CN108706641A - A kind of preparation method of ultra-thin sulfide nanometer sheet - Google Patents
A kind of preparation method of ultra-thin sulfide nanometer sheet Download PDFInfo
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- CN108706641A CN108706641A CN201810809623.1A CN201810809623A CN108706641A CN 108706641 A CN108706641 A CN 108706641A CN 201810809623 A CN201810809623 A CN 201810809623A CN 108706641 A CN108706641 A CN 108706641A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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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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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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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
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
Abstract
The present invention relates to a kind of preparation methods of two-dimensional material, refer in particular to a kind of preparation method of ultra-thin sulfide nanometer sheet.The present invention utilizes liquid nitrogen up-stripping method, simply and effectively prepares the single layer of a large amount of high quality or the two-dimentional platinum sulfide nano flake of few layer, and reduce the cost of precious metal catalyst.
Description
Technical field
The present invention relates to a kind of atomic level two dimension platinum sulfide preparation of sections methods, belong to the energy and material science and technology
Field.
Background technology
In recent years, two-dimensional material by researchers extensive concern.By the way that the thickness of bulk material is reduced to original
Sub- thickness, local atomic arrangement such as ligancy, bond distance, bond angle and atomic disorder degree will be changed.The thin thickness of atom will be led
More exposed interior atoms are caused, and should be easy to induce the formation of various defects, this is undoubtedly to the physico of them
Learning property has significant impact.Due to the strong quantum confinement of superhigh specific surface area, ultrathin and Two-dimensional electron, these atoms are thin
2D materials can not only show the intrinsic property of bulk material, but also generate the new property not available for corresponding bulk material
Matter.
There are many type of two-dimensional material, can substantially be divided into following several classes.Simplest structure and graphene and six side's nitrogen
Change boron, the transition metal curing with the sandwich structure that single-layer metal atom and two layers of chalcogen or halogen are formed
Object (TMDs) (such as PtS2, PtSe2, MoS2And WS2) and metal halide (PbI2And MgBr2)；It is more to embody laminated structure
Layered metal oxide (such as MnO of sample2And MnO3), all these compounds being bonded with planar structure, each diversity are all
It can be removed by way of from bottom to top as nanoscale twins.Since the single layer two-dimensional material obtained after stripping has many spies standby
Property, the stripping of two-dimensional material and be applied to develop an effective way of new material and application.
The thin 2D materials of atom can provide more surface-active sites.With the continuous deepening of research, many researchs
Person has found, the radial dimension of two-dimensional material is to the electricity of material, optically and thermally property has apparent influence.Work as two-dimensional material
Radial dimension be reduced to 20nm and it is following when be classified as quantum dot, catalysis reaction normally tends to the original for being happened at low ligancy
On son, such as edge, angle or terrace atom, it is typically considered surface-active site.The research of two dimension quantum dot belongs to just at present
Stage phase, many potential properties need further to be researched and developed.Therefore it develops a kind of with universality, high yield and method
The two-dimentional quantum dot preparation method of green is still urgently to be resolved hurrily.
Invention content
The present invention relates to a kind of preparation method of atomic level two dimension sulfide nano flake, to existing preparation method into
Row improvement simply and effectively prepares the two dimension vulcanization of the single layer or few layer of a large amount of high quality using liquid nitrogen up-stripping method
Platinum nano flake, and reduce the cost of precious metal catalyst.
The preparation method of ultra-thin two-dimension sulfide proposed by the present invention, includes the following steps：
(1) it is 1 according to Pt/S atomic ratios:2 ratio weighs platinum powder and sulphur powder, the two is transferred to after evenly mixing respectively
In quartz test tube and carry out sealing treatment.
(2) quartz ampoule sealed up for safekeeping in step (1) is placed in tube furnace, in the environment of 600 DEG C -900 DEG C of set temperature
Heating heating is carried out, grey black PtS is obtained by the reaction using chemical vapour deposition technique2Solid powder.
(3) quartz ampoule of step (2) is subjected to open pipe and takes out grey black PtS2Solid.
(4) the grey black PtS in step (3) is weighed2Solid is added in the mixed solvent and obtains mixed liquor；The mixing is molten
Agent is made of water and solvent；Solvent is acetone, isopropanol, tetrahydrofuran, methanol, chloroform, n-butanol, hexane, dimethylbenzene
One of with acetonitrile.
The grey black PtS2The mass volume ratio of solid powder and mixed solvent is 0.02-0.5g：10-200mL, it is described
The volume ratio of in the mixed solvent, solvent and water is 1：1-3：1；It is preferred that 2:1.
(5) mixed liquor of above-mentioned steps (4) is subjected to first time liquid nitrogen frozen processing, then ultrasonic stripping is carried out to mixed liquor
Processing, finally centrifuges, supernatant is taken to move in clean tube；Again after second of liquid nitrogen frozen is handled, freeze drier is utilized
It is ultra-thin sulfide nanometer sheet that device, which obtains dry solid,.
The first time liquid nitrogen frozen time is 1-4h, preferably 2h.
Second of liquid nitrogen frozen time is 10min, this processing is blocking just for the sake of freezing, and is conveniently obtained fluffy dry
Dry sample.
The ultrasound lift-off processing time is 2-12h, preferably 4h, power 100-200W.
The centrifugal rotational speed is 500-16500rpm, preferably 2000rpm.
(6) the ultra-thin sulfide nanometer sheet of above-mentioned steps (5) and support materials are subjected to ultrasonic mixing in ethanol solution,
The mass ratio of ultra-thin sulfide nanometer sheet and support materials is 0.0001-0.05:1, mixed solution is filtered, filtering is washed with water
Object, until removing remaining solvent；Filtrate is dry in air dry oven, obtain the two-dimentional platinum sulfide of single layer or few layer
Nanometer sheet compound.
The ultrasonic time is 1-4h；Drying temperature is 60 DEG C.
The PtS2It is preferably 0.005 with support materials mass ratio:1.
The support materials are mesoporous carbonitride, graphene, carbon pipe, carbon ball, zinc oxide, silica, aluminium oxide, oxidation
Iron, any one of manganese oxide or molecular sieve.
The present invention is by selecting volume ratio, liquid nitrogen frozen time, ultrasonic lift-off processing time and the centrifugation of solvent and water to turn
Speed obtains the PtS of high quality monolayer or few layer2Two-dimensional nano sheet material.
The PtS of single layer proposed by the present invention or few layer2Preparation method, its advantage is that：The method of the present invention can obtain height
The PtS of effect and high quality monolayer applied widely or few layer2Two-dimentional quanta point material, and preparation process is simple to operation simultaneously
And this process is not introduced into intractable solvent.The present invention can not only prepare the PtS of single layer or few layer2, while obtain with it is mesoporous
The compound that carbonitride is formed is in addition, single layer prepared by the present invention or the PtS for lacking layer2With excellent performance, such as the present invention
The PtS of the single layer being supported on mesoporous carbonitride or few layer that prepare2, the cost of precious metal catalyst is not only significantly reduced, also
With definitely Photocatalyzed Hydrogen Production performance.
Description of the drawings
Fig. 1 is the PtS of single layer prepared by the method for the present invention or few layer2Transmission electron microscope, it was demonstrated that synthesis nanometer thin
Piece.
Fig. 2 is the PtS of single layer prepared by the method for the present invention or few layer2Atomic force microscopy diagram；Pass through atomic force microscopy
Mirror characterization illustrates the PtS of single layer or few layer2Layer thickness be 0.781nm, mutually echoed with transmission plot, it was demonstrated that successfully synthesize nanometer thin
Piece.
Fig. 3 is the PtS of single layer prepared by the method for the present invention embodiment 4 or few layer2The mesoporous carbonitride of load, is being not added with platinum
Under conditions of carry out Photocatalyzed Hydrogen Production performance test.
Specific implementation mode
The embodiment of the method for the present invention introduced below：
Embodiment 1：
First, it is 1 according to Pt/S atomic ratios:Both platinum powder and sulphur powder are transferred to quartz test tube by 2 ratio after evenly mixing
In and carry out sealing treatment.The quartz ampoule sealed up for safekeeping is placed in tube furnace, heating is carried out in 600 DEG C of environment of set temperature and is added
Heat, reaction are completed to obtain pure grey black PtS2Solid powder.Take the grey black PtS of 0.005g260mL isopropanols are added in solid
With the mixed liquor (volume ratio of water：2:1) liquid nitrogen frozen, is carried out to the mixed liquor and handles 2h, and then ultrasonic stripping is carried out to it
4h is handled, 500rpm is finally centrifuged, takes supernatant to move to for use in clean tube.Freezing processing is carried out through liquid nitrogen again, when freezing
Between 10min, obtain dry solid.The mass ratio of ultra-thin sulfide nanometer sheet and mesoporous carbonitride is 0.005:1, it is molten in ethyl alcohol
Ultrasonic mixing is carried out in liquid, mixed solution is filtered, filtrate is washed with water, until removing remaining solvent；Filtrate is existed
It is dry in air dry oven, obtain the two dimension vulcanization nano sheets of platinum compound of single layer or few layer.
Embodiment 2：(compared with Example 1, we change stripping solvent)
First, it is 1 according to Pt/S atomic ratios:Both platinum powder and sulphur powder are transferred to quartz test tube by 2 ratio after evenly mixing
In and carry out sealing treatment.The quartz ampoule sealed up for safekeeping is placed in tube furnace, heating is carried out in 600 DEG C of environment of set temperature and is added
Heat, reaction are completed to obtain pure grey black PtS2Solid powder.Take the grey black PtS of 0.005g2Solid, be added 60mL acetone with
Mixed liquor (the volume ratio of water：2:1) liquid nitrogen frozen, is carried out to the mixed liquor and handles 2h, and then it is carried out at ultrasonic stripping
4h is managed, 500rpm is finally centrifuged, takes supernatant to move to for use in clean tube.Again freezing processing, cooling time are carried out through liquid nitrogen
10min obtains dry solid.The mass ratio of ultra-thin sulfide nanometer sheet and mesoporous carbonitride is 0.005:1, in ethanol solution
Middle carry out ultrasonic mixing filters mixed solution, filtrate is washed with water, until removing remaining solvent；By filtrate in drum
It is dry in wind drying box, obtain the two dimension vulcanization nano sheets of platinum compound of single layer or few layer.
The effect of embodiment 2 is better than embodiment 1, and it is more abundant to be mainly reflected in peeling effect, can remove thinner more
Ultra-thin vulcanization nano sheets of platinum.
Embodiment 3：(compared with Example 2, we change the volume ratio of solvent and water)
First, it is 1 according to Pt/S atomic ratios:Both platinum powder and sulphur powder are transferred to quartz test tube by 2 ratio after evenly mixing
In and carry out sealing treatment.The quartz ampoule sealed up for safekeeping is placed in tube furnace, heating is carried out in 600 DEG C of environment of set temperature and is added
Heat, reaction are completed to obtain pure grey black PtS2Solid powder.Take the grey black PtS of 0.005g2Solid, be added 60mL acetone with
Mixed liquor (the volume ratio of water：1:1) liquid nitrogen frozen, is carried out to the mixed liquor and handles 2h, and then it is carried out at ultrasonic stripping
4h is managed, 500rpm is finally centrifuged, takes supernatant to move to for use in clean tube.Again freezing processing, cooling time are carried out through liquid nitrogen
10min obtains dry solid.The mass ratio of ultra-thin sulfide nanometer sheet and mesoporous carbonitride is 0.005:1, in ethanol solution
Middle carry out ultrasonic mixing filters mixed solution, filtrate is washed with water, until removing remaining solvent；By filtrate in drum
It is dry in wind drying box, obtain the two dimension vulcanization nano sheets of platinum compound of single layer or few layer.
The effect of embodiment 3 is better than embodiment 1 but poor than embodiment 2, and peeling effect is than embodiment 1 more fully but than reality
It is poor to apply example 2.
Embodiment 4：(compared with Example 2, we change centrifugal speed)
First, it is 1 according to Pt/S atomic ratios:Both platinum powder and sulphur powder are transferred to quartz test tube by 2 ratio after evenly mixing
In and carry out sealing treatment.The quartz ampoule sealed up for safekeeping is placed in tube furnace, heating is carried out in 600 DEG C of environment of set temperature and is added
Heat, reaction are completed to obtain pure grey black PtS2Solid powder.Take the grey black PtS of 0.005g2Solid, be added 60mL acetone with
Mixed liquor (the volume ratio of water：2:1) liquid nitrogen frozen, is carried out to the mixed liquor and handles 2h, and then it is carried out at ultrasonic stripping
4h is managed, 2000rpm is finally centrifuged, takes supernatant to move to for use in clean tube.Again freezing processing, cooling time are carried out through liquid nitrogen
10min obtains dry solid.The mass ratio of ultra-thin sulfide nanometer sheet and mesoporous carbonitride is 0.005:1, in ethanol solution
Middle carry out ultrasonic mixing filters mixed solution, filtrate is washed with water, until removing remaining solvent；By filtrate in drum
It is dry in wind drying box, obtain the two dimension vulcanization nano sheets of platinum compound of single layer or few layer.
The effect of embodiment 4 is better than embodiment 2, and the mass ratio of 4 gained compound of embodiment is less than embodiment 2, but gained
The layer thickness of catalyst can obtain thinner vulcanization nano sheets of platinum, improve catalyst after optimization centrifugal speed centrifugation
Utilization ratio.
Embodiment 5-11
Other are same as Example 4, but remove solvent and be changed to tetrahydrofuran, methanol, chloroform, positive fourth respectively by acetone
Alcohol, hexane, dimethylbenzene and acetonitrile, effect are poorer than embodiment 4；But it is better than isopropanol.
Claims (9)
1. a kind of preparation method of ultra-thin sulfide nanometer sheet, which is characterized in that be as follows：
(1) it is 1 according to Pt/S atomic ratios:2 ratio weighs platinum powder and sulphur powder, the two is transferred to quartz after evenly mixing respectively
In test tube and carry out sealing treatment；
(2) quartz ampoule sealed up for safekeeping in step (1) is placed in tube furnace, is carried out in the environment of 600 DEG C -900 DEG C of set temperature
Heating heating, grey black PtS is obtained by the reaction using chemical vapour deposition technique2Solid powder；
(3) quartz ampoule of step (2) is subjected to open pipe and takes out grey black PtS2Solid；
(4) the grey black PtS in step (3) is weighed2Solid is added in the mixed solvent and obtains mixed liquor；The mixed solvent is by water
It is formed with solvent；Solvent is acetone, isopropanol, tetrahydrofuran, methanol, chloroform, n-butanol, hexane, dimethylbenzene and acetonitrile
One of；
(5) mixed liquor of above-mentioned steps (4) is subjected to first time liquid nitrogen frozen processing, then mixed liquor is carried out at ultrasonic stripping
Reason, finally centrifuges, supernatant is taken to move in clean tube；Again after second of liquid nitrogen frozen is handled, freeze-drying instrument is utilized
It is ultra-thin sulfide nanometer sheet to obtain dry solid.
2. a kind of preparation method of ultra-thin sulfide nanometer sheet as described in claim 1, which is characterized in that in step (4), institute
State grey black PtS2The mass volume ratio of solid powder and mixed solvent is 0.02-0.5g：10-200mL, the mixed solvent
In, the volume ratio of solvent and water is 1：1-3：1；The solvent is acetone.
3. a kind of preparation method of ultra-thin sulfide nanometer sheet as claimed in claim 2, which is characterized in that in step (4), institute
The volume ratio for stating solvent and water is 2：1.
4. a kind of preparation method of ultra-thin sulfide nanometer sheet as described in claim 1, which is characterized in that in step (5)；Institute
It is 1-4h to state liquid nitrogen frozen time first time；Second of liquid nitrogen frozen time is 10min；The ultrasound lift-off processing time
For 2-12h, power 100-200W；The centrifugal rotational speed is 500-16500rpm.
5. a kind of preparation method of ultra-thin sulfide nanometer sheet as claimed in claim 4, which is characterized in that in step (5)；Institute
It is 2h to state liquid nitrogen frozen time first time；The ultrasound lift-off processing time is 4h；The centrifugal rotational speed is 2000rpm.
6. the method for preparing nanometer sheet compound using ultra-thin sulfide nanometer sheet prepared by method as described in claim 1,
It is characterized in that, is as follows：Ultra-thin sulfide nanometer sheet and support materials are subjected to ultrasonic mixing in ethanol solution, surpassed
The mass ratio of thin sulfide nanometer sheet and support materials is 0.0001-0.05:1, mixed solution is filtered, filtering is washed with water
Object, until removing remaining solvent；Filtrate is dry in air dry oven, obtain the two-dimentional platinum sulfide of single layer or few layer
Nanometer sheet compound.
7. method as claimed in claim 6, which is characterized in that the ultrasonic time is 1-4h；Drying temperature is 60 DEG C.
8. method as claimed in claim 6, which is characterized in that the PtS2It is 0.005 with support materials mass ratio:1.
9. method as claimed in claim 6, which is characterized in that the support materials are mesoporous carbonitride, graphene, carbon
Pipe, carbon ball, zinc oxide, silica, aluminium oxide, iron oxide, any one of manganese oxide or molecular sieve.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109879321A (en) * | 2019-04-15 | 2019-06-14 | 南京邮电大学 | A kind of preparation method of semiconductor phase molybdenum disulfide nano sheet |
| CN111068735A (en) * | 2019-12-27 | 2020-04-28 | 电子科技大学 | PtS quantum dot/g-C3N4Nanosheet composite photocatalyst and preparation method thereof |
| CN113967475A (en) * | 2021-09-15 | 2022-01-25 | 江苏大学 | Preparation method and application of plasma-induced layered nickel-cobalt bimetallic hydroxide photocatalytic material |
| CN114950490A (en) * | 2022-05-12 | 2022-08-30 | 江苏大学 | Preparation of aminated monolayer PtS by plasma technology 2 Method for quantum dots |
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| WO2016133570A1 (en) * | 2015-02-20 | 2016-08-25 | Northeastern University | Low noise ultrathin freestanding membranes composed of atomically-thin 2d materials |
| CN108046250A (en) * | 2017-12-22 | 2018-05-18 | 江苏大学 | A kind of preparation method of two-dimensional material |
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| KR101563231B1 (en) * | 2014-12-19 | 2015-10-26 | 성균관대학교산학협력단 | Nanosheet-inorganic layered porous nanostructure, and preparing method of the same |
| WO2016133570A1 (en) * | 2015-02-20 | 2016-08-25 | Northeastern University | Low noise ultrathin freestanding membranes composed of atomically-thin 2d materials |
| CN108046250A (en) * | 2017-12-22 | 2018-05-18 | 江苏大学 | A kind of preparation method of two-dimensional material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879321A (en) * | 2019-04-15 | 2019-06-14 | 南京邮电大学 | A kind of preparation method of semiconductor phase molybdenum disulfide nano sheet |
| CN111068735A (en) * | 2019-12-27 | 2020-04-28 | 电子科技大学 | PtS quantum dot/g-C3N4Nanosheet composite photocatalyst and preparation method thereof |
| CN113967475A (en) * | 2021-09-15 | 2022-01-25 | 江苏大学 | Preparation method and application of plasma-induced layered nickel-cobalt bimetallic hydroxide photocatalytic material |
| CN113967475B (en) * | 2021-09-15 | 2023-09-22 | 江苏大学 | Preparation method and application of plasma-induced layered nickel-cobalt double-metal hydroxide photocatalytic material |
| CN114950490A (en) * | 2022-05-12 | 2022-08-30 | 江苏大学 | Preparation of aminated monolayer PtS by plasma technology 2 Method for quantum dots |
| CN114950490B (en) * | 2022-05-12 | 2023-10-13 | 江苏大学 | Preparation of amination monolayer PtS by plasma technology 2 Quantum dot method |
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