CN111204796A - Method for preparing SnS2 nano material by direct current arc plasma - Google Patents

Method for preparing SnS2 nano material by direct current arc plasma Download PDF

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CN111204796A
CN111204796A CN201911236871.2A CN201911236871A CN111204796A CN 111204796 A CN111204796 A CN 111204796A CN 201911236871 A CN201911236871 A CN 201911236871A CN 111204796 A CN111204796 A CN 111204796A
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vacuum tube
tube furnace
furnace
direct current
sulfur
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CN111204796B (en
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黄昊
吴爱民
刘强
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Dalian University of Technology
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Dalian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—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
    • 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
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
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Abstract

The invention discloses a method for preparing SnS by using direct current arc plasma2A method of nanomaterials comprising the steps of: preparing pure Sn nano particles as a precursor by using a direct current arc plasma technology, and uniformly mixing the pure Sn nano particles and elemental sulfur in a molar ratio of 1: 3.7-1: 6.7 to obtain a tin-sulfur mixture; transferring the tin-sulfur mixture into a sealed cavity, vacuumizing the sealed cavity, sealing, and placing the sealed cavity into a vulcanization reaction furnace body for vulcanization reaction at the temperature of 400 ℃; after the vulcanization reaction is finished, cooling to room temperature along with the furnace, grinding the sample in the sealed cavity, removing sulfur, and then cooling to room temperature along with the furnace to obtain SnS2And (3) nano materials. The invention uses pure tin and elemental sulfur as the tin source and the sulfur source, has low cost, and obtains SnS by controlling the tin and sulfur dosage, the reaction time and the reaction temperature2The nano material is simple to operate and suitable for commercial production.

Description

SnS (stannum sulfide) preparation by direct current arc plasma2Method for preparing nano material
Technical Field
The invention belongs to the field of a preparation method of a nano material, and particularly relates to a method for preparing SnS by using direct current arc plasma2A method of preparing a nanomaterial.
Background
Because the transition metal sulfide of the graphene-like structure has a proper forbidden band structure, the utilization of the transition metal sulfide to light can utilize solar energy more than that of a photocatalyst responding to ultraviolet light. The visible light response sulfide is mainly CdS and ZnS. The most discussed CdS, although very good under lightThe chromium element has toxicity and the CdS can be corroded by light under the irradiation of light. ZnS itself does not respond optically in the visible and needs to be doped with metals or complexed with other semiconductors to act as a photocatalyst. And MoS2The semiconductor performance is also poor due to the high electron-hole recombination rate.
SnS2The photocatalyst is an effective visible light response N-type photocatalyst, the band gap of the photocatalyst is 2.18-2.244eV, the photocatalyst has the characteristics of no toxicity, relative cheapness and chemical stability, and the appropriate conduction band level and the appropriate band gap of the photocatalyst enable the photocatalyst to be widely applied to the field of photocatalysis. Based on the above consideration, SnS2Is a good visible light catalytic material. Currently synthesized SnS2The method is a hydrothermal reaction and a solvothermal method, the used tin source and sulfur source are mainly organic matters, the operation of the chemical combination process is complex, and byproducts are generated in the reaction process. So that the SnS is prepared by cheap materials and a simple method2Nanomaterials still need further exploration.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for synthesizing SnS by using a direct current arc plasma method2A method of preparing a nanomaterial. The invention takes pure tin blocks and elemental sulfur as a tin source and a sulfur source, and prepares the flaky SnS by controlling the conditions of the molar ratio of tin to sulfur, the reaction temperature, the reaction time and the like2And (3) nano materials. The technical means adopted by the invention are as follows:
SnS prepared by direct current arc plasma2A method of nanomaterials comprising the steps of:
s1, preparing pure Sn nanoparticles as a precursor from the pure tin block by a direct current arc plasma technology, and uniformly mixing the pure Sn nanoparticles and elemental sulfur in a molar ratio of 1: 3.7-1: 6.7 to obtain a tin-sulfur mixture;
s2, transferring the tin-sulfur mixture into a sealed cavity, vacuumizing the sealed cavity, sealing, and placing the sealed cavity into a vulcanization reaction furnace body for vulcanization reaction at the temperature of 400 ℃;
s3, after the vulcanization reaction is finished, cooling to room temperature along with the furnace, and sealingGrinding the sample in the sealed cavity, desulfurizing, and cooling to room temperature along with the furnace to obtain SnS2And (3) nano materials.
The purity of the pure tin block is 99.99 percent, and the elemental sulfur is of analytical grade;
the molar ratio of the precursor to the elemental sulfur is 1:4 or 1: 6.7.
In the step S2, the sealing chamber is a long-necked glass bottle, the long-necked glass bottle is vacuumized and a small amount of shielding gas is introduced to make the vacuum degree in the long-necked glass bottle be 0.03MPa, and then the neck of the long-necked glass bottle is blown off for sealing;
the device for the vulcanization reaction is a tubular furnace or a stainless steel reaction kettle;
preserving the heat for 1.75 to 2.5 hours after reaching the vulcanization reaction temperature;
the temperature rise speed in the vulcanization reaction process is 10 ℃/min.
In step S3, the desulfurization apparatus is a vacuum tube furnace;
the desulfurization treatment comprises the following specific steps:
placing the ground sample in a vacuum tube furnace, vacuumizing the vacuum tube furnace, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, heating the vacuum tube furnace to 200 ℃ at the speed of 10 ℃/min, preserving the temperature for 2h, cooling the vacuum tube furnace to room temperature, vacuumizing the vacuum tube furnace when the furnace temperature is increased to 90 ℃, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, vacuumizing the vacuum tube furnace every 20min, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, and cooling the vacuum tube furnace to 90 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses pure tin and elemental sulfur as the tin source and the sulfur source, has low cost, and obtains SnS by controlling the tin and sulfur dosage, the reaction time and the reaction temperature2The nano material is simple to operate and suitable for commercial production; specifically, hydrothermal or solvothermal reaction is a simple and efficient method for preparing nanomaterials, and then the hydrothermal or solvothermal method is currently utilizedOrganic matters are used for reaction, the operation of the reaction process is complex, and byproducts are generated in the reaction process; the invention adopts cheap pure tin block and elemental sulfur as reaction raw materials, and obtains SnS with higher purity by simple operations such as reasonable proportion, reaction time, temperature and the like2And (3) nano materials.
Based on the reasons, the invention can be widely popularized in the fields of nano material preparation methods 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 to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows a direct current arc plasma method for preparing SnS according to an embodiment of the present invention2A flow diagram of a method of nanomaterials;
FIG. 2 shows SnS prepared in example 1 of the present invention2An X-ray diffraction pattern of the nanomaterial;
FIG. 3 shows SnS prepared in example 1 of the present invention2Scanning electron microscope images of the nano materials;
FIG. 4 shows SnS prepared in example 1 of the present invention2Ultraviolet-visible absorption spectrum of the nano material.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in FIG. 1Showing, a method for preparing SnS by direct current arc plasma2The method for preparing the nano material comprises the following specific steps:
preparing simple substance Sn nano particles from blocky pure tin (99.99%) by a direct current arc plasma technology (controlling the main parameter of direct current arc: current is 70A) as a precursor, and uniformly mixing 0.3518g of the simple substance Sn nano particles prepared in the previous step with 0.3798g of simple substance sulfur (the molar ratio of the simple substance Sn nano particles to the simple substance sulfur is 1: 4); and then adding the glass bottle into a long-neck glass bottle, vacuumizing the long-neck glass bottle, introducing a small amount of Ar gas serving as protective gas to enable the vacuum degree in the long-neck glass bottle to be 0.03MPa, and burning the neck of the long-neck glass bottle to be fused and sealed by using an alcohol blast burner. Transferring the long-neck glass bottle into a stainless steel reaction kettle, heating to 400 ℃ at the speed of 10 ℃/min, and preserving heat for 2 h. After the reaction is finished, naturally cooling to room temperature, grinding uniformly, transferring the quartz boat into a vacuum tube furnace, placing the quartz boat into the vacuum tube furnace, vacuumizing the vacuum tube furnace, introducing a small amount of Ar gas as protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, heating the vacuum tube furnace to 200 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and then cooling to room temperature along with the furnace to obtain SnS2And (3) a nano material, wherein when the furnace temperature is increased to 90 ℃, the vacuum tube furnace is vacuumized and a small amount of Ar gas is introduced so that the vacuum degree in the vacuum tube furnace is 0.03MPa, and then the vacuum tube furnace is vacuumized and a small amount of Ar gas is introduced every 20min so that the vacuum degree in the vacuum tube furnace is 0.03MPa until the furnace is cooled to 90 ℃.
As shown in fig. 2, the molar ratio Sn: the XRD diffraction pattern of the tin sulfide powder prepared by heating and vulcanizing S is more than or equal to 1:4 at 400 ℃ for 2h and then carrying out desulphurization treatment is shown, and the pattern shows that the ratio of Sn: when the molar ratio of S is more than or equal to 1:4, the generated product is pure phase SnS2And the card is completely matched with the PDF card (23-0677).
As shown in FIG. 3, the prepared tin sulfide nano-powder is irregular and flaky, the thickness is about 50nm, and the tin sulfide nano-flake is agglomerated.
As shown in fig. 4, the spectroscopic apparatus was tested: lambda 950 ultraviolet visible near infrared spectrophotometer;
the measuring method comprises the following steps: fixing a sample on a quartz glass slide, and scanning and measuring by using an integrating sphere diffuse reflection absorption spectrum mode;
as can be seen from the figure, a distinct intrinsic absorption edge occurs around the wavelength 550 nm.
Example 2
As shown in figure 1, a direct current arc plasma preparation SnS2The method for preparing the nano material comprises the following specific steps:
preparing simple substance Sn nano particles from blocky pure tin (99.99%) by a direct current arc plasma technology (controlling the main parameter of direct current arc: current is 70A) as a precursor, and uniformly mixing 0.2043g of the simple substance Sn nano particles prepared in the previous step with 0.3688g of simple substance sulfur (the molar ratio of the simple substance Sn nano particles to the simple substance sulfur is 1: 6.7); and then adding the glass bottle into a long-neck glass bottle, vacuumizing the long-neck glass bottle, introducing a small amount of Ar gas serving as protective gas to enable the vacuum degree in the long-neck glass bottle to be 0.03MPa, and burning the neck of the long-neck glass bottle to be fused and sealed by using an alcohol blast burner. Transferring the long-neck glass bottle into a stainless steel reaction kettle, heating to 400 ℃ at the speed of 10 ℃/min, and preserving heat for 2 h. After the reaction is finished, naturally cooling to room temperature, then uniformly grinding (grinding the blocky or agglomerated powder into powder), transferring the powder into a quartz boat, placing the quartz boat into a vacuum tube furnace, vacuumizing the vacuum tube furnace, introducing a small amount of Ar gas serving as protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, heating the vacuum tube furnace to 200 ℃ at the speed of 10 ℃/min, preserving the temperature for 2 hours, and then cooling to room temperature along with the furnace to obtain SnS2And (3) a nano material, wherein when the furnace temperature is increased to 90 ℃, the vacuum tube furnace is vacuumized and a small amount of Ar gas is introduced so that the vacuum degree in the vacuum tube furnace is 0.03MPa, and then the vacuum tube furnace is vacuumized and a small amount of Ar gas is introduced every 20min so that the vacuum degree in the vacuum tube furnace is 0.03MPa until the furnace is cooled to 90 ℃.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (4)

1. SnS prepared by direct current arc plasma2A method of producing nanomaterials comprising the steps of:
s1, preparing pure Sn nanoparticles as a precursor from the pure tin block by a direct current arc plasma technology, and uniformly mixing the pure Sn nanoparticles and elemental sulfur in a molar ratio of 1: 3.7-1: 6.7 to obtain a tin-sulfur mixture;
s2, transferring the tin-sulfur mixture into a sealed cavity, vacuumizing the sealed cavity, sealing, and placing the sealed cavity into a vulcanization reaction furnace body for vulcanization reaction at the temperature of 400 ℃;
s3, after the vulcanization reaction is finished, cooling to room temperature along with the furnace, grinding the sample in the sealed cavity, carrying out desulphurization treatment, then cooling to room temperature along with the furnace to obtain SnS2And (3) nano materials.
2. Direct current arc plasma preparation SnS according to claim 12The method of the nanometer material is characterized in that the purity of the pure tin block is 99.99 percent, and the elemental sulfur is of analytical grade;
the molar ratio of the precursor to the elemental sulfur is 1:4 or 1: 6.7.
3. Direct current arc plasma preparation SnS according to claim 12The method for preparing the nano material is characterized in that in the step S2, the sealing cavity is a long-neck glass bottle, the long-neck glass bottle is vacuumized and is filled with a small amount of protective gas to enable the vacuum degree in the long-neck glass bottle to be 0.03MPa, and then the neck of the long-neck glass bottle is burned off and sealed;
the device for the vulcanization reaction is a tubular furnace or a stainless steel reaction kettle;
preserving the heat for 1.75 to 2.5 hours after reaching the vulcanization reaction temperature;
the temperature rise speed in the vulcanization reaction process is 10 ℃/min.
4. Direct current arc plasma preparation SnS according to claim 12The method of nano-materials, wherein in step S3, the device for desulfurization treatment is a vacuum tube furnace;
the desulfurization treatment comprises the following specific steps:
placing the ground sample in a vacuum tube furnace, vacuumizing the vacuum tube furnace, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, heating the vacuum tube furnace to 200 ℃ at the speed of 10 ℃/min, preserving the temperature for 2h, cooling the vacuum tube furnace to room temperature, vacuumizing the vacuum tube furnace when the furnace temperature is increased to 90 ℃, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, vacuumizing the vacuum tube furnace every 20min, introducing a small amount of protective gas to ensure that the vacuum degree in the vacuum tube furnace is 0.03MPa, and cooling the vacuum tube furnace to 90 ℃.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109748318A (en) * 2019-02-18 2019-05-14 云南锡业集团（控股）有限责任公司研发中心 A kind of preparation method of stannous sulfide

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109748318A (en) * 2019-02-18 2019-05-14 云南锡业集团（控股）有限责任公司研发中心 A kind of preparation method of stannous sulfide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CESAR D. POMAR ET.AL: ""Synthesis of SnS and ZnS Hollow Microarchitectures Decorated with Nanostructures and Their Photocatalytic", 《MATERIALS SCIENCE INC. NANOMATERIALS & POLYMERS》 *
谷泽宇等: ""多壁纳米碳管约束二硫化锡作为锂离子电池负极的电化学行为"", 《物理化学学报》 *

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