CN108383149A - Cu2The nanocrystalline controllable synthesis methods of S - Google Patents
Cu2The nanocrystalline controllable synthesis methods of S Download PDFInfo
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- CN108383149A CN108383149A CN201810442960.1A CN201810442960A CN108383149A CN 108383149 A CN108383149 A CN 108383149A CN 201810442960 A CN201810442960 A CN 201810442960A CN 108383149 A CN108383149 A CN 108383149A
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- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to nanocrystalline synthesis fields, more particularly to Cu2Controllable synthesis method nanocrystalline S, this method is using CuNWs as presoma, using mercaptan as sulphur source, is added or is added without borine tert-butylamine, by controlling reaction temperature and reaction process to obtain the Cu of different crystalline phases2S is nanocrystalline.After technical solution disclosed in this invention, the copper sulfide (I) with specific crystalline phase, including but not limited to cubic phase, hexagonal phase, monoclinic phase crystalline phase can be controllably synthesized;So as to provide infrastructural support as semi-conducting material especially renewable hydrogen oxygen fuel cell material for copper sulfide.Meanwhile method disclosed by the invention, without expensive solvent and harsh reaction condition, production cost is lower, is easy to industrialization promotion.
Description
Technical field
The present invention relates to nanocrystalline synthesis fields, and in particular to Cu2Synthesis nanocrystalline S, more particularly to Cu2S nanometers
Brilliant controllable synthesis method.
Background technology
The crisis of energy shortage threatens always the survival and development of the mankind, while the environmental pollution caused by industrial production
Problem also constitutes huge puzzlement to the survival and development of the mankind, in order to solve environment and the energy this two large problems, scientists
Always in the storage device of extensive concern and discovery with energy conversion and excellent performance.Renewable hydrogen oxygen fuel cell is considered
It is efficient, clean energy conversion device, there is very high application value and application it is expected, therefore in the field of business causes extensively
Concern.
Nanometer semiconductor structure is considered as a kind of can be used for having for emerging activity and integrated nano-scale device
The building block of future.Therefore, the research of nanometer semiconductor structure becomes the hot fields for attracting researcher at present.
In the suitable semiconductor nano material of selection, 2 points are primarily to consider, first, the semiconductor nano needs to have
There is the semiconductor structure of appropriate band gap;Second, the semiconductor nano material is preferably able to be environmental-friendly and recyclable.
Copper sulfide (I) is a candidate for meeting above-mentioned requirements, vitreous copper (Cu2S be a kind of volume band gap it is) 1.2eV
P-type semiconductor, in solar cell, the application fields such as cold cathode and nanotube switch have a wide range of applications.Zhou seminars
Et al. successfully synthesized the uniform Cu of appearance and size2S nanometer sheets, experiment are closed using the synthetic method of vulcanization polyisoprene
At going out sheet Cu2The thickness of S only has 1.2nm, ultra-thin Cu2S nanometer sheets show excellent optical property, multiple with nanofiber
After conjunction, TiO is significantly improved2The performance of photolysis water hydrogen.
But still have problems with:It is most of about Cu2The research of the synthesis of S is with high boiling polynary
It is carried out in alcoholic solvent such as ethylene glycol, because they are at elevated temperatures by Cu2+It is reduced to Cu+Ability.However, these are molten
Agent is expensive, and the use of them is compared with water more difficult.
Invention content
The goal of the invention of the present invention is to provide that a kind of cost is relatively low, is easy to brilliant controllable of copper sulphide nano of industrialization promotion
Synthetic method.
In order to achieve the above-mentioned object of the invention, the invention discloses a kind of Cu2The nanocrystalline controllable synthesis methods of S, this method with
CuNWs is presoma, using mercaptan as sulphur source, is added or is added without borine tert-butylamine, by controlling reaction temperature and react into
Journey is to obtain the Cu of different crystalline phases2S is nanocrystalline.
It is further preferred that the mercaptan is n-octyl mercaptan either n- dodecyl mereaptan.
When using n-octyl mercaptan for sulphur source, cubic phase Cu is obtained2S is nanocrystalline;When using lauryl mercaptan for sulphur source, obtain
Obtain hexagonal phase Cu2S is nanocrystalline;When using lauryl mercaptan monoclinic phase Cu is obtained for sulphur source, and when borine tert-butylamine is added2S nanometers
It is brilliant.
Wherein, the controlling reaction temperature refers to 5-8 DEG C of min-1Rate is warming up to 260-280 DEG C.
Reaction process refers to, including two stages of temperature rise period and holding stage;Wherein the temperature rise period uses 5-8 DEG C
min-1Rate is warming up to 260-280 DEG C, enters holding stage, the insulation reaction 100- at 260-280 DEG C after reaching 260-280 DEG C
150min。
And it is further preferred that temperature rise period and holding stage are completed in sand-bath.
The adding proportion of the presoma and mercaptan is:Cu NWs 0.5mmol, mercaptan 10mL.
When added with borine tert-butylamine complex compound, additive amount 400mg.
Wherein it is further preferred that with 6 DEG C of min-1Rate heats up.
It is further preferred that 280 DEG C are warming up to, and in 280 DEG C of insulation reactions.
In another preferred technical solution, the insulation reaction 60min at 280 DEG C.
As another preferred technical solution, it is original that the preparation method invention additionally discloses presoma CuNWs, which is with CuCl,
Material, with octadecylene (ODE) for solvent, lauryl amine (DDA) is reducing agent, and oleic acid (OA) is protective agent, using temperature programming, is formed
The linear structure of Cu nanocrystals.
It is further preferred that the preparation method of presoma CuNWs is:After CuCl, oleic acid and octadecylene are mixed, it is placed in sand
In bath, 280 DEG C is warming up to using temperature programmed control stage, and reducing agent lauryl amine is added in the moment for being warming up to 280 DEG C, protected
Temperature reaction, obtains red brown solid.
It is further preferred that the heating of described program temperature control stage specifically includes temperature programmed control with 7 DEG C of min-1Rate by
Room temperature rises to 85 DEG C, rises to 150 DEG C after keeping the temperature 20min, 280 DEG C are risen to after keeping the temperature 10min.
Further, in the present invention further preferably after reducing agent lauryl amine is added, 20min is kept the temperature.
It is further preferred that further including the mixed solvent purified product with normal heptane and absolute ethyl alcohol.
When product is the linear structure of Cu nanocrystals, the mixed volume ratio of normal heptane and absolute ethyl alcohol is 3:1.
When product is the cubic phase of Cu nanocrystals, hexagonal phase or monocline phase structure, normal heptane and absolute ethyl alcohol
Mixed volume ratio is 1:1.
After technical solution disclosed in this invention, the copper sulfide (I) with specific crystalline phase can be controllably synthesized, is wrapped
Include but be not limited to cubic phase, hexagonal phase, monoclinic phase crystalline phase;So as to for copper sulfide it is especially renewable as semi-conducting material
Hydrogen-oxygen fuel cell material provides infrastructural support.Meanwhile method disclosed by the invention is without expensive solvent and harsh reaction
Condition, production cost is lower, is easy to industrialization promotion.
Description of the drawings
The TEM figures that Fig. 1 is the CuNWs synthesized in the embodiment of the present invention 1.
The EDS figures that Fig. 2 is the CuNWs synthesized in the embodiment of the present invention 1.
Fig. 3 is the XRD diagram of the Cu NWs synthesized in the embodiment of the present invention 1.
Fig. 4 is the Cu synthesized in the embodiment of the present invention 2 to embodiment 42(wherein a figures are the TEM figures of nanocrystalline three crystalline phases of S
Cubic phase;B figures are hexagonal phase;C figures are monoclinic phase).
Fig. 5 is the monoclinic phase Cu synthesized in the embodiment of the present invention 42The Mapping of nanocrystalline three crystalline phases of S schemes.
Fig. 6 is the Cu synthesized in the embodiment of the present invention 2 to embodiment 42The XRD diagram of nanocrystalline three crystalline phases of S.
Specific implementation mode
In order to better understand the present invention, we in conjunction with specific embodiments further explain the present invention below
It states.
Embodiment 1
Weigh 99.1mg CuCl, add the raw material into dry capacity be 250mL three neck round bottom in, then with shifting
Liquid rifle draws 0.5mL oleic acid, and 5mL octadecylenes are placed in flask, are transferred to sand-bath, temperature programmed control is with 7 DEG C of min-1Rate by room
Temperature rises to 85 DEG C, and 150 DEG C are risen to after keeping the temperature 20min, and 280 DEG C of (heating moment addition 4.5mL 12 are risen to after keeping the temperature 10min
Amine), it reacts and terminates after keeping the temperature 60min.Reactor is cooled to 50~60 DEG C, and supernatant liquid is outwelled after cooling down slightly, is added a small amount of
Normal heptane disperses bottom of bottle solid.With normal heptane and absolute ethyl alcohol (3:1) it is saturating to be washed till supernatant clarification for mixed solution centrifuge washing
It is bright, obtain red brown solid vacuum drying.
Sample is measured, testing result figure is as shown in Figure 1-Figure 3.It can be seen that according to Fig. 1-Fig. 3:What is obtained consolidates
Body is the linear structure of Cu, and diameter is about 20nm.Its essential element is Cu, and product purity is higher.By Search Match
Software compares, and determines that it is Cu nano wires (JCPDS-1-1241) to obtain product.
The experiment of embodiment 2- embodiments 4 is carried out using obtained copper nano-wire in embodiment 1 as raw material.
It should be noted that can also use the copper nano-wire that other methods obtain for raw material in embodiment 2 to embodiment 4
Carry out the preparation of copper sulphide nano crystalline substance.
Embodiment 2
32mg (0.5mmol) Cu NWs are weighed, the three neck round bottom that dry capacity is 250mL is added the raw material into
In, then draw eight mercaptan of 10mL with liquid-transfering gun and be placed in flask, three neck round bottom is transferred in sand-bath by ultrasonic disperse, journey
With 6 DEG C of min under sequence temperature control-1Rate be warming up to 280 DEG C, and keep the temperature 60min at this temperature, reaction terminates.Wait for reactor certainly
It is so cooled to room temperature, centrifuges solid.By solid normal heptane and absolute ethyl alcohol (1:1) black is obtained after mixed solution washing
Product is dried in vacuum overnight in vacuum drying chamber.
Product is detected, as shown in fig. 4 a, the Cu which obtains2The nanocrystalline crystal forms of S are cubic phase.
Embodiment 3
At room temperature, 32mg (0.5mmol) CuNWs, 400mg borine tert-butylamine complex compound (BTBC) is weighed, is added raw materials into
In the three neck round bottom for being 250mL to dry capacity, then draws 10mL lauryl mercaptans with liquid-transfering gun and be placed in flask, ultrasound
Dispersion, three neck round bottom is transferred in sand-bath, with 6 DEG C of min under temperature programmed control-1Rate be warming up to 280 DEG C, and it is warm herein
After the lower heat preservation 60min of degree, reaction terminates.It waits for reactor cooled to room temperature, centrifuges solid.By solid normal heptane and
Absolute ethyl alcohol (1:1) black product is obtained after mixed solution washing, is dried in vacuum overnight in vacuum drying chamber.
Product is detected, as illustrated in fig. 4 c, the Cu which obtains2The nanocrystalline crystal forms of S are monoclinic phase.
Embodiment 4
32mg (0.5mmol) Cu NWs are weighed, the three neck round bottom that dry capacity is 250mL is added the raw material into
In, then draw 10mL lauryl mercaptans with liquid-transfering gun and be placed in flask, three neck round bottom is transferred in sand-bath by ultrasonic disperse,
With 6 DEG C of min under temperature programmed control-1Rate be warming up to 280 °, and keep the temperature 60min at this temperature, reaction terminates.Wait for reactor certainly
It is so cooled to room temperature, centrifuges solid.By solid normal heptane and absolute ethyl alcohol (1:1) black is obtained after mixed solution washing
Product is dried in vacuum overnight in vacuum drying chamber.
Product is detected, as shown in Figure 4 b, the Cu which obtains2The nanocrystalline crystal forms of S are hexagonal phase.
Embodiment 5
The product obtained in embodiment 2 to embodiment 4 is subjected to XRD detections, testing result is as shown in Figure 6.
From fig. 6 it can be seen that three products can all compare out Cu2Crystal form card nanocrystalline S, from the point of view of diffraction maximum,
Cubic phase Cu2Crystallization degree nanocrystalline S is best, and miscellaneous peak is few, and diffraction maximum is apparent, and peak width is relatively narrow.
Embodiment 6
Take monoclinic phase Cu2The nanocrystalline progress Mapping Scanning Detctions of S, testing result is as shown in figure 5, as seen from Figure 5
Cu elements and S Elemental redistributions are uniform in product.
The above is the specific implementation mode of the present invention.It should be pointed out that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (10)
1.Cu2The nanocrystalline controllable synthesis methods of S, it is characterised in that:This method, using mercaptan as sulphur source, adds using CuNWs as presoma
Enter or be added without borine tert-butylamine, by controlling reaction temperature and reaction process to obtain the Cu of different crystalline phases2S nanometers
It is brilliant.
2. Cu according to claim 12The nanocrystalline controllable synthesis methods of S, it is characterised in that:The mercaptan is n-octyl mercaptan
Either n- dodecyl mereaptan.
3. Cu according to claim 12The nanocrystalline controllable synthesis methods of S, it is characterised in that:The controlling reaction temperature
Refer to 5-8 DEG C of min-1Rate is warming up to 260-280 DEG C.
4. Cu according to claim 12The nanocrystalline controllable synthesis methods of S, it is characterised in that:Reaction process refers to, including rises
Two stages of thermophase and holding stage;Wherein the temperature rise period uses 5-8 DEG C of min-1Rate is warming up to 260-280 DEG C, reaches
Enter holding stage, the insulation reaction 100-150min at 260-280 DEG C after 260-280 DEG C.
5. Cu according to claim 12The nanocrystalline controllable synthesis methods of S, it is characterised in that:The presoma and mercaptan
Adding proportion is:CuNWs 0.5mmol, mercaptan 10mL.
6. Cu according to claim 52The nanocrystalline controllable synthesis methods of S, it is characterised in that:When added with borine tert-butylamine
When complex compound, additive amount 400mg.
7. Cu according to claim 12The nanocrystalline controllable synthesis methods of S, it is characterised in that:The preparation side of presoma CuNWs
Method is using CuCl as raw material, and with octadecylene (ODE) for solvent, lauryl amine (DDA) is reducing agent, and oleic acid (OA) is protective agent, profit
With temperature programming, the linear structure of Cu nanocrystals is formed.
8. Cu according to claim 72The nanocrystalline controllable synthesis methods of S, it is characterised in that:The preparation side of presoma CuNWs
Method is:It after CuCl, oleic acid and octadecylene are mixed, is placed in sand-bath, 280 DEG C is warming up to using temperature programmed control stage, and
Reducing agent lauryl amine is added in the moment for being warming up to 280 DEG C, insulation reaction obtains red brown solid.
9. Cu according to claim 72The nanocrystalline controllable synthesis methods of S, it is characterised in that:Described program temperature control is interim
Heating specifically includes temperature programmed control with 7 DEG C of min-1Rate rise to 85 DEG C by room temperature, rise to 150 DEG C after keeping the temperature 20min, heat preservation
280 DEG C are risen to after 10min.
10. the Cu according to claim 1 or 82The nanocrystalline controllable synthesis methods of S, it is characterised in that:Further include using normal heptane
With the mixed solvent purified product of absolute ethyl alcohol;When product is the linear structure of Cu nanocrystals, normal heptane and absolute ethyl alcohol
Mixed volume ratio be 3:1;When product is the cubic phase of Cu nanocrystals, hexagonal phase or monocline phase structure, normal heptane with
The mixed volume ratio of absolute ethyl alcohol is 1:1.
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Cited By (4)
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CN110302808A (en) * | 2018-12-28 | 2019-10-08 | 江南大学 | A kind of rodlike molybdenum disulfide/copper sulphide nano composite material and preparation method |
CN111847499A (en) * | 2020-08-07 | 2020-10-30 | 北京理工大学 | Method for preparing copper-doped cadmium sulfide nanosheet based on ion exchange reaction |
CN112279306A (en) * | 2020-10-21 | 2021-01-29 | 南京晓庄学院 | Optimization method of sulfide nanocrystal, Sn-S-Co nanocrystal and optimized product thereof |
CN115318306A (en) * | 2022-02-22 | 2022-11-11 | 哈尔滨工业大学 | Cu-rich material 2 S nanocrystal modified Cu nanosheet and preparation method and application thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110302808A (en) * | 2018-12-28 | 2019-10-08 | 江南大学 | A kind of rodlike molybdenum disulfide/copper sulphide nano composite material and preparation method |
CN111847499A (en) * | 2020-08-07 | 2020-10-30 | 北京理工大学 | Method for preparing copper-doped cadmium sulfide nanosheet based on ion exchange reaction |
CN111847499B (en) * | 2020-08-07 | 2021-06-08 | 北京理工大学 | Method for preparing copper-doped cadmium sulfide nanosheet based on ion exchange reaction |
CN112279306A (en) * | 2020-10-21 | 2021-01-29 | 南京晓庄学院 | Optimization method of sulfide nanocrystal, Sn-S-Co nanocrystal and optimized product thereof |
CN112279306B (en) * | 2020-10-21 | 2021-07-06 | 南京晓庄学院 | Optimization method of sulfide nanocrystal, Sn-S-Co nanocrystal and optimized product thereof |
CN115318306A (en) * | 2022-02-22 | 2022-11-11 | 哈尔滨工业大学 | Cu-rich material 2 S nanocrystal modified Cu nanosheet and preparation method and application thereof |
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