CN106830056A - One kind prepares SnS using hydro-thermal method2The method of hexagonal nanometer sheet - Google Patents
One kind prepares SnS using hydro-thermal method2The method of hexagonal nanometer sheet Download PDFInfo
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- CN106830056A CN106830056A CN201710007439.0A CN201710007439A CN106830056A CN 106830056 A CN106830056 A CN 106830056A CN 201710007439 A CN201710007439 A CN 201710007439A CN 106830056 A CN106830056 A CN 106830056A
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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
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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
- C01P2002/70—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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- 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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
Abstract
SnS is prepared using hydro-thermal method the invention discloses one kind2The method of hexagonal nanometer sheet, reactant presoma sulfur-containing compound, soluble pink salt, highly basic, deionized water are added in reactor successively first, it is stirred at room temperature to reactant dissolving, then reactor sealing is put into vacuum drying oven, 180 240 DEG C are reacted 10 days 12 hours, naturally cool to room temperature；Precipitation and separation is finally washed, SnS is obtained final product2Hexagonal nanometer sheet.The present invention is simple to operate, without equipment requirement；The various solvents for being used are environmentally friendly, produced without high toxic material, with low cost, are adapted to commercially produce.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of preparation method of stannic disulfide, specifically one kind uses water
Hot method prepares SnS2The method of hexagonal nanometer sheet.
Background technology
The energy is the basis of economic development, is also primary condition for the survival of mankind, with the rapid hair of modern industry
Exhibition, the demand to the energy is more and more.The use of conventional fossil energy can discharge substantial amounts of carbon dioxide and some harmful gas
Body, serious destruction is caused to environment, therefore, restructure the use of energy, finding renewable new energy has turned into the necessary face of the whole mankind
To primary problem.Regenerative resource is the conventional fossil energy most efficient method of substitution.Regenerative resource is roughly divided into wind energy,
Solar energy, underground heat, tide energy etc..In the above-mentioned energy, solar energy is most potential as main stream, and its reserves extremely enriches,
Can continuously outwardly good fortune penetrates energy, be the maximum energy that can be developed in the world now, it is renewable far above other
The energy, can meet worldwide energy consumption.It is well known that solar energy cleanliness without any pollution, can be with to the exploitation of solar energy
Environmental protection.The most promising opto-electronic conversion to realize solar energy in the mode using solar energy, i.e., using photogenic voltage
Solar energy is directly changed into electric energy by effect.
SnS2Used as a kind of n-type semiconductor, broadband energy gap is about 2.1eV, and band gap wider is allowed to good light
Learn and electrology characteristic；Meanwhile, it is two kinds of element earth rich contents of Sn, S, nontoxic, therefore SnS2 is a kind of very promising film
Solar cell material.
In Chinese patent " SnS2Nanometer piece preparation method, ultra-thin SnS2In nanometer sheet and its application "（CN 104362000A）
One kind is disclosed based on Oleic Acid System, after Xi Yuan and different sulphur sources are directly added into Oleic Acid System, by controlling to add
The method that the type of sulphur source obtains different-thickness stannic disulphide nano slice, so as to prepare two under normal pressure and relatively low temperature
The method of artificial gold nanometer sheet.Still the method does reaction dissolvent using organic solvent in the method, and nanometer sheet is difficult to control, and uses
The method of cheap and simple prepares the SnS with controllable appearance and reduced size in aqueous2Nano material is still one very big
Challenge.Chinese patent " Hydrothermal Synthesiss SnS2The method of nano material "（CN 103373742A）Middle use sour environment system
Product dispersiveness is not fine, SnS after reaction2Can reunite, and this method can overcome this shortcoming using alkaline environment.
The content of the invention
For above-mentioned technical problem of the prior art, SnS is prepared using hydro-thermal method the invention provides one kind2Hexagonal is received
The method of rice piece, described this use hydro-thermal method prepares SnS2The method of hexagonal nanometer sheet will solve method of the prior art
The SnS of preparation2Hexagonal nanometer sheet poor dispersion, is susceptible to the technical problem reunited.
SnS is prepared using hydro-thermal method the invention provides one kind2The method of hexagonal nanometer sheet, comprises the following steps：
1) reactant presoma sulfur-containing compound, pink salt, highly basic and deionized water, described reactant presoma Containing Sulfur are weighed
The material ratio of compound, pink salt, highly basic and deionized water is 20-70 mmol：10-30mmol：2-15 g：5-50 mL；Wherein：Institute
State sulfur-containing compound and may be selected from any one in thiocarbamide, sulphur powder, vulcanized sodium, thioacetic acid, sodium thiosulfate or thioacetamide；
The highly basic is selected from any one in NaOH, potassium hydroxide, rubidium hydroxide or cesium hydroxide；
2) reactant presoma sulfur-containing compound, pink salt, highly basic and deionized water are added in reactor successively, at room temperature
Stir 5-30 min to reactant presoma dissolving；
3) and then by reactor sealing put into vacuum drying oven, 180-240 DEG C is reacted -10 days 12 hours, naturally cools to room
Temperature；
4) precipitation and separation is finally washed, SnS is obtained final product2Hexagonal nanometer sheet；
Further, described pink salt is selected from any one in stannic chloride pentahydrate or stannous chloride.
Further, the temperature of the hydrothermal synthesis reaction is 180~200 DEG C.
Further, the time of the hydrothermal synthesis reaction is 1-7 days.
Preparation principle of the invention is as follows：
Sn4+ + 4OH− → SnO2 + 2H2O
NH2CSNH2 + 2H2O → 2NH3 + H2S + CO2
SnO2 + 2H2S → SnS2 + 2H2O.
The present invention is using Hydrothermal Synthesiss SnS2Method, it is with low cost, by controlling the consumption of reactant, reaction temperature and anti-
The controllable SnS of available size between seasonable2Nano material.
The present invention is compared with prior art, and its technological progress is significant.The present invention is simple to operate, without equipment requirement；Institute
The various solvents for using are environmentally friendly, produced without high toxic material, with low cost, are adapted to commercially produce.
Brief description of the drawings
Fig. 1 is the SnS that the embodiment of the present invention 1 is prepared using hydro-thermal method2The X ray diffracting spectrum of hexagonal nanometer sheet, from figure
In it can be seen that its crystallinity preferably, and without other dephasigns.
Fig. 2 is the SnS that the embodiment of the present invention 1 is prepared using hydro-thermal method2The crystal structure figure of hexagonal nanometer sheet, SnS2It is layer
Six side CdI of shape2Crystal structure, metal tin atom forms laminated structure in the way of hexagonal closs packing, is embedded in by sulphur atom
With between the laminated structure that hexagonal closs packing is formed.
The SnS that Fig. 3 is prepared for this hair embodiment 1 using hydro-thermal method2The scanning electron microscope (SEM) photograph of hexagonal nanometer sheet, it is in the length of side
4 μm of average out to, the hexagonal structure that 1 μm of thickness average out to.
Fig. 4 is the SnS that the embodiment of the present invention 1 is prepared using hydro-thermal method2Hexagonal nanometer sheet is scattered in the ultraviolet suction in ethanol
Receive figure.
Specific embodiment
Embodiment 1：
The g sulphur powders of reactant presoma 0.64,5.22 g stannic chloride pentahydrates, 10 g potassium hydroxide, 20 mL are gone successively first
Ionized water is added in reactor, and 5 min to reactant presoma are stirred at room temperature, and is then put into reactor sealing true
200 DEG C are reacted 3 days in empty baking oven, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal nanometer sheet.
Embodiment 2：
The g sulphur powders of reactant presoma 2.24,10.52 g stannic chloride pentahydrates, 8 g potassium hydroxide, 30 mL are gone successively first
Ionized water is added in reactor, 15 min is stirred at room temperature and is dissolved to reactant presoma thing, then seals reactor
Put into vacuum drying oven 230 DEG C to react 5 days, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal is received
Rice piece.
Embodiment 3：
The g sulphur powders of reactant presoma 1.25,3.50 g stannic chloride pentahydrates, 15 g potassium hydroxide, 40 mL are gone successively first
Ionized water is added in reactor, 30 min is stirred at room temperature and is dissolved to reactant presoma thing, then seals reactor
Put into vacuum drying oven 190 DEG C to react 6 days, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal is received
Rice piece.
Embodiment 4：
First successively by the g sulphur powders of reactant presoma 2.20,4.65 g stannic chloride pentahydrates, 2 g potassium hydroxide, 50 mL go from
Sub- water is added in reactor, and 10 min are stirred at room temperature to the dissolving of reactant presoma thing, then seals reactor
Put into vacuum drying oven 220 DEG C to react 2 days, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal is received
Rice piece.
Embodiment 5：
The g sulphur powders of reactant presoma 1.56,8.67 g stannic chloride pentahydrates, 12 g potassium hydroxide, 25 mL are gone successively first
Ionized water is added in reactor, 20 min is stirred at room temperature and is dissolved to reactant presoma thing, then seals reactor
Put into vacuum drying oven 180 DEG C to react 1 day, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal is received
Rice piece.
Embodiment 6：
First successively by the g sulphur powders of reactant presoma 0.8,3.65 g stannic chloride pentahydrates, 6 g potassium hydroxide, 5 mL deionizations
Water is added in reactor, 18 min is stirred at room temperature and is dissolved to reactant presoma thing, is then put into reactor sealing
240 DEG C are reacted 3 days in vacuum drying oven, naturally cool to room temperature, finally wash precipitation and separation, obtain final product SnS2Hexagonal nanometer sheet.
Embodiment 7：
First successively by the g of reactant presoma 0.92（20-70 mmol）Sulphur powder, 4.32 g stannic chloride pentahydrates, 12 g hydrogen-oxygens
Change potassium, 28 mL deionized waters to be added in reactor, 22 min to reactant presoma thing dissolving are stirred at room temperature, then
Reactor sealing is put into vacuum drying oven into 200 DEG C to react 12 hours, room temperature is naturally cooled to, precipitation and separation is finally washed,
Obtain final product SnS2Hexagonal nanometer sheet.
Claims (4)
1. it is a kind of that SnS is prepared using hydro-thermal method2The method of hexagonal nanometer sheet, it is characterised in that comprise the following steps：
1）Weigh reactant presoma sulfur-containing compound, pink salt, highly basic and deionized water, described reactant presoma Containing Sulfur
The material ratio of compound, pink salt, highly basic and deionized water is 20-70 mmol：10-30mmol：2-15 g：5-50 mL；Wherein：Institute
State sulfur-containing compound and may be selected from any one in thiocarbamide, sulphur powder, vulcanized sodium, thioacetic acid, sodium thiosulfate or thioacetamide；
The highly basic is selected from any one in NaOH, potassium hydroxide, rubidium hydroxide or cesium hydroxide；
2）Reactant presoma sulfur-containing compound, pink salt, highly basic and deionized water are added in reactor successively, at room temperature
Stir 5-30 min to reactant presoma dissolving；
3）Then reactor sealing is put into vacuum drying oven, 180-240 DEG C is reacted -10 days 12 hours, naturally cools to room
Temperature；
4）Precipitation and separation is finally washed, SnS is obtained final product2Hexagonal nanometer sheet.
2. according to claim 1 a kind of using hydro-thermal method preparation SnS2The method of hexagonal nanometer sheet, it is characterised in that：Institute
The pink salt stated is selected from any one in stannic chloride pentahydrate or stannous chloride.
3. according to claim 1 a kind of using hydro-thermal method preparation SnS2The method of hexagonal nanometer sheet, it is characterised in that：Institute
The temperature for stating hydrothermal synthesis reaction is 180~200 DEG C.
4. according to claim 1 a kind of using hydro-thermal method preparation SnS2The method of hexagonal nanometer sheet, it is characterised in that：Institute
The time for stating hydrothermal synthesis reaction is 1-7 days.
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| CN201710007439.0A CN106830056A (en) | 2017-01-05 | 2017-01-05 | One kind prepares SnS using hydro-thermal method2The method of hexagonal nanometer sheet |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107437615A (en) * | 2017-07-05 | 2017-12-05 | 东莞中汽宏远汽车有限公司 | High-capacity lithium battery negative pole and preparation method thereof and lithium battery |
| CN107686125A (en) * | 2017-08-29 | 2018-02-13 | 哈尔滨工业大学 | A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive |
| CN109900745A (en) * | 2019-02-25 | 2019-06-18 | 吉林大学 | One kind being based on rGO-SnS2The NO of compound2Sensor and preparation method thereof |
| CN110526281A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of synthesis stannic disulfide |
| CN111285397A (en) * | 2020-03-09 | 2020-06-16 | 西安工业大学 | Method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets |
| CN111484070A (en) * | 2020-04-21 | 2020-08-04 | 天津理工大学 | Synthetic preparation method of semi-metal phase tin disulfide |
| CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
| CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
| CN113484302A (en) * | 2021-07-01 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | SnS with capillary effect2Microsphere SERS substrate and preparation method and application thereof |
| CN114195181A (en) * | 2021-11-26 | 2022-03-18 | 长沙理工大学 | Preparation method of micron-sized copper sulfide nanosheet and copper sulfide nanosheet |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103373742A (en) * | 2013-07-05 | 2013-10-30 | 上海交通大学 | Method for hydrothermal synthesis of SnS2 nano-materials |
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Patent Citations (1)
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| CN103373742A (en) * | 2013-07-05 | 2013-10-30 | 上海交通大学 | Method for hydrothermal synthesis of SnS2 nano-materials |
Non-Patent Citations (2)
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| LINGYAN WANG等: "High-rate performance of SnS2 nanoplates without carbon-coating as anode material for lithium ion batteries", 《ELECTROCHIMICA ACTA》 * |
| YONG CAI ZHANG等: "Size-Tunable Hydrothermal Synthesis of SnS2 Nanocrystals with High Performance in Visible Light-Driven Photocatalytic Reduction of Aqueous Cr(VI)", 《ENVIRON. SCI. TECHNOL.》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107437615A (en) * | 2017-07-05 | 2017-12-05 | 东莞中汽宏远汽车有限公司 | High-capacity lithium battery negative pole and preparation method thereof and lithium battery |
| CN107686125A (en) * | 2017-08-29 | 2018-02-13 | 哈尔滨工业大学 | A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive |
| CN107686125B (en) * | 2017-08-29 | 2019-07-02 | 哈尔滨工业大学 | A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive |
| CN109900745A (en) * | 2019-02-25 | 2019-06-18 | 吉林大学 | One kind being based on rGO-SnS2The NO of compound2Sensor and preparation method thereof |
| CN110526281B (en) * | 2019-08-26 | 2021-08-24 | 浙江工业大学 | Method for synthesizing tin disulfide |
| CN110526281A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of synthesis stannic disulfide |
| CN111285397A (en) * | 2020-03-09 | 2020-06-16 | 西安工业大学 | Method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets |
| CN111484070A (en) * | 2020-04-21 | 2020-08-04 | 天津理工大学 | Synthetic preparation method of semi-metal phase tin disulfide |
| CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
| CN111517363B (en) * | 2020-04-30 | 2022-04-01 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
| CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
| CN113484302A (en) * | 2021-07-01 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | SnS with capillary effect2Microsphere SERS substrate and preparation method and application thereof |
| CN114195181A (en) * | 2021-11-26 | 2022-03-18 | 长沙理工大学 | Preparation method of micron-sized copper sulfide nanosheet and copper sulfide nanosheet |
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