CN110627125B - Method for synthesizing manganese sulfide and lead sulfide nanorod with core-shell structure - Google Patents
Method for synthesizing manganese sulfide and lead sulfide nanorod with core-shell structure Download PDFInfo
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- 239000002073 nanorod Substances 0.000 title claims abstract description 58
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000011258 core-shell material Substances 0.000 title claims abstract description 44
- 229910052981 lead sulfide Inorganic materials 0.000 title claims abstract description 36
- 229940056932 lead sulfide Drugs 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- 239000002243 precursor Substances 0.000 claims description 23
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 20
- 230000035484 reaction time Effects 0.000 claims description 13
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 12
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 12
- 229940099607 manganese chloride Drugs 0.000 claims description 12
- 235000002867 manganese chloride Nutrition 0.000 claims description 12
- 239000011565 manganese chloride Substances 0.000 claims description 12
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 10
- 239000011572 manganese Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 229910052748 manganese Inorganic materials 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 239000002159 nanocrystal Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910052745 lead Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- -1 cadmium chalcogenide Chemical class 0.000 description 2
- 238000005341 cation exchange Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- PGWMQVQLSMAHHO-UHFFFAOYSA-N sulfanylidenesilver Chemical class [Ag]=S PGWMQVQLSMAHHO-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- 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
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
- C01P2004/86—Thin layer coatings, i.e. the coating thickness being less than 0.1 time the particle radius
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Abstract
The invention relates to a method for synthesizing a manganese sulfide and lead sulfide core-shell structure nanorod, which belongs to the technical field of nano material preparation. The method has the advantages of simple process, controllable product morphology and aspect ratio, high repeatability and the like, and the prepared sample has high phase purity, good crystallinity and uniform particle size distribution.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing a manganese sulfide and lead sulfide nanorod with a core-shell structure.
Background
In recent years, nano materials have become the main research content of basic research and technical application, and are mainly applied to the fields of catalysis, solar cells, light emitting diodes, lithium ion batteries, gas sensitivity and the like. As an important magnetic semiconductor material, Mn-based chalcogenide semiconductor materials (MnX, X ═ S, Se, Te) exhibit various important optical, magnetic, and electron transport properties, which depend on their crystal structures. In particular, MnX semiconductors are antiferromagnetic semiconductor materials, so their magnetic arrangement is also very specific. To date, cationic exchange has become an extremely versatile method for obtaining a wide variety of materials and nanostructures in various post-synthesis treatments of colloidal nanocrystals. One notable example in this direction is partial cation exchange by which preformed nanocrystals can be converted into alloy nanocrystals or into various types of nano-heterostructures having a core/shell, segmented or striped structure. In ionic nanocrystals, cation exchange reactions have been used by using different goldBy substitution of cations within the nanocrystal lattice by ions to alter the composition of the material, e.g. by adding a small molar excess of Ag to cadmium chalcogenide nanocrystals (CdS, CdSe, CdTe)+The cations completely convert them into corresponding silver-sulfur compounds, or via a portion of Cu+Exchange-synthesized CdS-Cu2And (4) synthesizing the S nanorod heterostructure. However, so far, no report has been made on the structure of the preparation of manganese sulfide lead sulfide core-shell nanorods (in which the average length of the nanorods is about 52nm and the diameter is about 20 nm).
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method overcomes the problems and defects in the background technology, provides a method for synthesizing the nanorod with the manganese sulfide and lead sulfide core-shell structure, and regulates the thickness of the core shell of the nanorod by controlling the reaction time.
The invention takes manganese chloride, thioacetamide and lead chloride as raw materials, oleylamine, oleic acid and octadecene as ligands, and adopts a solvothermal method to synthesize a manganese sulfide and lead sulfide core-shell structure nanorod, and the specific technical scheme is as follows:
a method for synthesizing manganese sulfide and lead sulfide nanorod with a core-shell structure is carried out in a Schinker (Schlenk) system under the protection of nitrogen; comprises the following steps:
1) preparing a precursor solution of manganese sulfide, adding anhydrous manganese chloride and oleylamine into a three-necked bottle in a glove box, heating to 140 ℃ under the protection of nitrogen, completely dissolving manganese chloride powder to obtain a transparent manganese chloride solution with the concentration of 0.125M, keeping the transparent manganese chloride solution at the temperature of 140 ℃ for 20 minutes, heating the solution to 300 ℃, injecting an oleylamine solution of thioacetamide with the concentration of 0.5M after the temperature is stabilized, cooling the solution after the molar ratio of the manganese chloride to the thioacetamide is 1:1, cleaning and centrifuging the solution after 30 minutes to obtain manganese sulfide nanorods of the wurtzite, drying the sample in a freezing vacuum machine, mixing the manganese sulfide nanorods of the wurtzite with octadecene according to the mass-volume ratio of 1mg/mL, and heating to 100 ℃ to obtain the precursor solution of the manganese sulfide;
2) preparing a precursor solution of lead chloride, putting the lead chloride into a mixed solution of oleylamine and octadecene with the volume ratio of 1:4, and heating the mixed solution to 120 ℃ in an oil bath pot to completely dissolve the lead chloride to obtain the precursor solution of the lead chloride with the concentration of 0.023M;
3) performing hot injection reaction, namely injecting oleic acid into the precursor solution of the manganese sulfide in the step 1) at 100 ℃, keeping the temperature for 10 minutes, and then dropwise adding the precursor solution of the lead chloride in the step 2), wherein the volume ratio of the precursor solution of the manganese sulfide to the precursor solution of oleic acid to lead chloride is 10:1: 10; and then keeping for 10-30 minutes to obtain the manganese sulfide and lead sulfide core-shell structure nanorod.
In the preparation process, the thickness of the shell of the product can be adjusted by controlling the reaction time after the thermal injection, and the reaction is carried out for 10 minutes after the precursor solution of lead chloride is dropwise added, so as to obtain the core-shell structure nanorod with the shell thickness of 2 nm; or reacting for 30 minutes to obtain the core-shell structure nanorod with the shell thickness of 5 nm.
In step 1), the temperature is raised to 300 ℃, and the temperature raising rate is preferably 2.5 ℃/min.
Has the advantages that:
the method for preparing the manganese sulfide and lead sulfide core-shell nanorod structure has the advantages that: the prepared sample has high phase purity, good crystallinity and uniform particle size distribution; the preparation method has the advantages of simple process, controllable product appearance and aspect ratio, high repeatability and the like. Has the potential of large-scale production.
Drawings
FIG. 1 is a transmission electron microscope image of manganese sulfide nanorods to wurtzite prepared in example 1.
FIG. 2 is a high resolution electron microscope image of the manganese sulfide nanorods to wurtzite prepared in example 1.
FIG. 3 is a transmission electron microscope image of the core-shell nanorod structure of manganese sulfide and lead sulfide prepared in example 1 when the reaction time is 10 minutes.
FIG. 4 is a distribution diagram of manganese (Mn) elements of the manganese sulfide and lead sulfide core-shell nanorod structure prepared in example 1 when the reaction time is 10 minutes.
FIG. 5 is a distribution diagram of sulfur (S) elements of the manganese sulfide and lead sulfide core-shell nanorod structure prepared in example 1 when the reaction time is 10 minutes.
FIG. 6 is a distribution diagram of lead (Pb) elements of manganese sulfide and lead sulfide core-shell nanorod structures prepared in example 1, when the reaction time is 10 minutes.
FIG. 7 is an energy spectrum of the core-shell nanorod structure of manganese sulfide and lead sulfide prepared in example 1 when the reaction time is 10 minutes.
FIG. 8 is a transmission electron microscope image of the core-shell nanorod structures of manganese sulfide and lead sulfide prepared in example 2 when the reaction time is 30 minutes.
FIG. 9 is a distribution diagram of manganese (Mn) elements of the manganese sulfide and lead sulfide core-shell nanorod structure prepared in example 2 when the reaction time is 30 minutes.
FIG. 10 is a distribution diagram of sulfur (S) elements of the manganese sulfide and lead sulfide core-shell nanorod structure prepared in example 2 when the reaction time is 30 minutes.
FIG. 11 is a distribution diagram of lead (Pb) elements of manganese sulfide and lead sulfide core-shell nanorod structures prepared in example 2, when the reaction time is 30 minutes.
FIG. 12 is an energy spectrum of the core-shell nanorod structure of manganese sulfide and lead sulfide prepared in example 2 when the reaction time is 30 minutes.
Detailed Description
The invention will now be described in more detail with reference to the following examples, in which the reagents are, unless otherwise specified, commercially available products and are used without further purification.
Example 1 Synthesis of core-shell nanorod structures with relatively thin manganese sulfide and lead sulfide obtained by reaction for 10 minutes
The synthesis of the core-shell nanorod structure of thinner manganese sulfide and lead sulfide is carried out in a Schinker (Schlenk) system, the synthesis process needs nitrogen protection, and the specific synthesis process is as follows: firstly, preparing 0.5mmol/mL oleylamine solution of thioacetamide in a glove box at room temperature, filling 0.063g of manganese chloride and 4mL of oleylamine into a three-neck bottle, plugging two side ports of the three-neck bottle by rubber plugs, connecting a middle port to a Schlenk system, inserting a thermocouple into the liquid level from one side of the three-neck bottle, stirring and heating to 140 ℃ for 20 minutes to obtain clear transparent solution with the concentration of 0.125mmol/mL, then raising the temperature to 300 ℃ at the speed of 2.5 ℃/minute, injecting 1mL and 0.5mmol/mL oleylamine solution of thioacetamide when the temperature is stable, changing the solution into pink, cooling the solution after 30 minutes, washing with toluene and acetone, centrifuging, and repeating for 3 times to obtain the manganese sulfide nano rod of the wurtzite. The samples were dried in a freeze vacuum. 0.0323g of lead chloride is put into a 20mL weighing bottle, 1mL of oleylamine and 4mL of octadecene are added, and the mixture is heated to 120 ℃ in an oil bath kettle to completely dissolve the lead chloride, so that a precursor solution with the concentration of 0.03mmol/mL of lead chloride is obtained. Adding 0.005g of dried manganese sulfide nanorod sample of wurtzite and 5mL of octadecene solution into a 50mL three-necked bottle, and then connecting the three-necked bottle into a Hirak system to raise the temperature to 100 ℃ to obtain a precursor solution of manganese sulfide. And after the temperature is stable, injecting 0.5mL of oleic acid, keeping the temperature for 10 minutes, then dropwise injecting the precursor solution of lead chloride into a three-necked bottle, and reacting for 10 minutes to obtain the thinner nanorod core-shell structure.
The TEM image of the wurtzite manganese sulfide nanorods prepared in this example is shown in FIG. 1, and the average length of the manganese sulfide nanorods is about 52nm and the average diameter is about 20 nm. FIG. 2 is a high resolution electron microscope picture of the manganese sulfide nanorod, showing that the nanorod is a single crystal. FIG. 3 is a transmission electron microscope image of a core-shell nanorod structure of manganese sulfide and lead sulfide, and it can be seen that the shell thickness of the prepared sample is about 2 nm. FIGS. 4 to 6 are element distribution diagrams of a manganese sulfide and lead sulfide core-shell nanorod structure, showing that Mn, S and Pb elements are uniformly distributed to form the manganese sulfide and lead sulfide nanorod core-shell structure. FIG. 7 is a spectrum diagram of a core-shell nanorod structure of manganese sulfide and lead sulfide, which shows that the sample contains Mn, S and Pb elements, and the elemental composition content chart of FIG. 7 shows that the synthesized material is a core-shell nanorod structure of manganese sulfide and lead sulfide.
Example 2 Synthesis of core-shell nanorod structure of manganese sulfide and lead sulfide obtained by reaction for 30 minutes
The preparation process of the precursor and the use amount of each reactant are the same as those in example 1, and finally, the precursor solution of lead chloride is dropwise injected into a three-necked bottle, and then the reaction is carried out for 30 minutes to obtain a thicker nanorod core-shell structure.
The transmission electron microscope image of the core-shell nanorod structure of manganese sulfide and lead sulfide prepared in this example is shown in fig. 8, where the average length of the core-shell nanorod structure of manganese sulfide and lead sulfide is about 52nm, the average diameter is about 20nm, and the shell thickness is about 5 nm. FIGS. 9 to 11 are element distribution diagrams of the core-shell structure of the manganese sulfide and lead sulfide nanorods, showing that Mn, S and Pb elements are uniformly distributed to form the core-shell structure of the manganese sulfide and lead sulfide nanorods. FIG. 12 is a spectrum diagram of a core-shell nanorod structure of manganese sulfide and lead sulfide, which shows that the sample contains Mn, S and Pb elements, and the elemental composition content chart of FIG. 12 shows that the synthesized material is a core-shell nanorod structure of manganese sulfide and lead sulfide.
Claims (2)
1. A method for synthesizing manganese sulfide and lead sulfide nanorod with a core-shell structure is carried out in a Hirak system under the protection of nitrogen; comprises the following steps:
1) preparing a precursor solution of manganese sulfide, adding anhydrous manganese chloride and oleylamine into a three-necked bottle in a glove box, heating to 140 ℃ under the protection of nitrogen, completely dissolving manganese chloride powder to obtain a transparent manganese chloride solution with the concentration of 0.125M, keeping the transparent manganese chloride solution at the temperature of 140 ℃ for 20 minutes, heating the solution to 300 ℃ at the speed of 2.5 ℃/minute, injecting an oleylamine solution of thioacetamide with the concentration of 0.5M after the temperature is stable, cooling the solution, cleaning and centrifuging after the molar ratio of the manganese chloride to the thioacetamide is 1:1, obtaining manganese sulfide nanorods of the wurtzite, drying a sample in a freezing vacuum machine, mixing the manganese sulfide nanorods of the wurtzite and octadecene according to the mass-volume ratio of 1mg/mL, heating to 100 ℃ to obtain a precursor solution of the manganese sulfide;
2) preparing a precursor solution of lead chloride, putting the lead chloride into a mixed solution of oleylamine and octadecene with the volume ratio of 1:4, and heating the mixed solution to 120 ℃ in an oil bath pot to completely dissolve the lead chloride to obtain the precursor solution of the lead chloride with the concentration of 0.03M;
3) performing hot injection reaction, namely injecting oleic acid into the precursor solution of the manganese sulfide in the step 1) at 100 ℃, keeping the temperature for 10 minutes, and then dropwise adding the precursor solution of the lead chloride in the step 2), wherein the volume ratio of the precursor solution of the manganese sulfide to the precursor solution of oleic acid to lead chloride is 10:1: 10; and then keeping for 10-30 minutes to obtain the manganese sulfide and lead sulfide core-shell structure nanorod.
2. The method for synthesizing the nanorod with the core-shell structure of manganese sulfide and lead sulfide as claimed in claim 1, wherein in step 3), the thickness of the shell of the product is adjusted by controlling the reaction time after thermal injection, and after dropwise adding a precursor solution of lead chloride, the reaction is carried out for 10 minutes to obtain the nanorod with the core-shell structure and the shell thickness of 2 nm; or reacting for 30 minutes to obtain the core-shell structure nanorod with the shell thickness of 5 nm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830445A (en) * | 2009-12-15 | 2010-09-15 | 河南大学 | Novel method for synthetizing inorganic nanocrystal by taking acetylacetone as raw material |
| CN102036909A (en) * | 2008-03-24 | 2011-04-27 | 加利福尼亚大学董事会 | Composite nanorods with distinct regions |
| CN102942224A (en) * | 2012-11-10 | 2013-02-27 | 吉林大学 | Synthesis method for rock salt mine MnS nano-cuboid superlattice |
| CN105271135A (en) * | 2015-10-23 | 2016-01-27 | 吉林大学 | Method for preparing nanocrystalline with one-dimensional manganese selenide / manganese sulfide core/shell heterostructure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102036909A (en) * | 2008-03-24 | 2011-04-27 | 加利福尼亚大学董事会 | Composite nanorods with distinct regions |
| CN101830445A (en) * | 2009-12-15 | 2010-09-15 | 河南大学 | Novel method for synthetizing inorganic nanocrystal by taking acetylacetone as raw material |
| CN102942224A (en) * | 2012-11-10 | 2013-02-27 | 吉林大学 | Synthesis method for rock salt mine MnS nano-cuboid superlattice |
| CN105271135A (en) * | 2015-10-23 | 2016-01-27 | 吉林大学 | Method for preparing nanocrystalline with one-dimensional manganese selenide / manganese sulfide core/shell heterostructure |
Non-Patent Citations (1)
| Title |
|---|
| Mn基硫族半导体纳米晶的合成、性质及在高压下相稳定性的研究;杨新一;《中国博士学位论文全文数据库 工程科技I辑》;20130815;第19页 * |
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