CN114950490A - Preparation of aminated monolayer PtS by plasma technology 2 Method for quantum dots - Google Patents
Preparation of aminated monolayer PtS by plasma technology 2 Method for quantum dots Download PDFInfo
- Publication number
- CN114950490A CN114950490A CN202210514527.0A CN202210514527A CN114950490A CN 114950490 A CN114950490 A CN 114950490A CN 202210514527 A CN202210514527 A CN 202210514527A CN 114950490 A CN114950490 A CN 114950490A
- Authority
- CN
- China
- Prior art keywords
- pts
- aminated
- monolayer
- quantum dots
- plasma
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002096 quantum dot Substances 0.000 title claims abstract description 35
- 239000002356 single layer Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005516 engineering process Methods 0.000 title claims abstract description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000002135 nanosheet Substances 0.000 claims abstract description 14
- 230000004888 barrier function Effects 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 41
- 239000010453 quartz Substances 0.000 claims description 40
- 239000007787 solid Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 238000009832 plasma treatment Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 17
- 239000010410 layer Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000005476 size effect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 2
- 230000004913 activation Effects 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000006228 supernatant Substances 0.000 description 8
- 238000005576 amination reaction Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000003841 Raman measurement Methods 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
- B01J27/045—Platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/87—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing platina group metals
- C09K11/873—Chalcogenides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- 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
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Combustion & Propulsion (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biophysics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the scientific and technical field of material preparation methods, and discloses a plasma technology for preparing aminated single-layer PtS 2 A method of quantum dots. Will initially be hexagonal PtS 2 The nanosheet utilizes plasma technologyTreating with ammonia gas atmosphere to form PtS with few aminated layers 2 The nanosheets are subjected to two-dimensional ultrasonic deep stripping and rapid smashing by a cell smashing machine to obtain single-layer aminated PtS 2 And (4) quantum dots. The invention aims to design and synthesize a monolayer aminated PtS with more active sites 2 The quantum dots have remarkable quantum effects mainly embodied in the aspects of surface effects, quantum size effects, dielectric confinement effects and the like. The material greatly shortens a light migration path, stimulates the mobility of charges, is beneficial to improving the adsorption performance, reducing the energy barrier of chemical reaction and promoting the separation and activation of charges in the catalysis process, and has better application in the catalysis field. The method has the advantages of high efficiency, innovation, economy, environmental protection and the like.
Description
Technical Field
The invention belongs to the scientific and technical field of material preparation methods, and particularly relates to an aminated single-layer PtS prepared by a plasma technology 2 A preparation method of quantum dots.
Background
Two-dimensional transition metal material PtS 2 It is believed to have a suitable bandgap, to have conductive properties, to be a narrow bandgap noble metal chalcogenide, stable 1T phase (octahedral) structure, with each Pt atom coordinated with 6S atoms, and adjacent layers bound by van der waals forces. PtS 2 The band gap of a single layer is about 1.6eV, and the band gap of a bulk body can reach 0.25eV along with the increase of the layer number, which is caused by strong interlayer interaction, and the property of the bulk body also changes along with the change of an energy band structure. PtS 2 Can be used in the fields of field effect transistors, photoelectric detectors, photocatalysis, high-performance hybrid electronic devices and the like.
The plasma is an ionized gaseous substance consisting of atoms after part of electrons are deprived and positive and negative ions generated after atomic groups are ionized, and the macroscopic electroneutral ionized gas with the dimension larger than the Debye length is a fourth state except solid, liquid and gas. A large number of reactive particles are present in the plasma and are able to react with the surface of the material in contact. Are often used to modify the surface of materials. The method for dielectric barrier discharge in plasma has the characteristics of mild treatment conditions, controllable reaction time, low energy consumption, simple operation and the like.
With two-dimensional transition metal material (PtS) 2 ) In the course of research, it was found that a few or a single layer of material could provide more surface active sites and quantum dots could be formed with decreasing radial dimensions. The quantum dots have obvious quantum effects mainly embodied in the aspects of surface effects, quantum size effects, dielectric confinement effects and the like. Can shorten mobility of photoexcited charges and increase the number of sheetsA surface active site. Thus inventing a single-layer PtS prepared by plasma technology 2 Quantum dots are the most important thing we want to do.
Disclosure of Invention
The invention adopts the plasma technology to treat PtS by introducing ammonia 2 The time, the reaction electric power, the two-dimensional ultrasonic peeling time, the cell crushing time and the centrifugal rotating speed of the plasma technology are used for obtaining the amination monolayer PtS prepared by the plasma technology 2 And (4) quantum dots.
Preparation of aminated monolayer PtS by plasma technology 2 The method of the quantum dot comprises the following specific steps:
(1) respectively weighing platinum powder and sulfur powder according to the Pt/S atomic ratio of 1:2, uniformly mixing the platinum powder and the sulfur powder, transferring the mixture into a quartz test tube, sealing the quartz test tube, then placing the quartz test tube into a tube furnace, heating the quartz test tube at the set temperature of 800-900 ℃, and obtaining gray black PtS by using a chemical vapor deposition method 2 Opening the tube to take out the solid powder for later use;
(2) weighing the gray black PtS in the step (1) 2 Dissolving the solid in ethanol, ultrasonically dripping on a quartz plate, drying, placing the quartz plate in a sealed discharge reactor, and generating plasma in a dielectric barrier discharge mode to treat PtS 2 Vacuum drying after plasma treatment to obtain NH 2 -PtS 2 Nanosheets;
(3) weighing NH in the step (2) 2 -PtS 2 Adding the nanosheet solid into a centrifuge tube, respectively adding into a mixed solution of isopropanol and deionized water, and shaking up;
(4) performing two-dimensional ultrasonic stripping on the mixed solution obtained in the step (3), then performing cell crushing on the mixed solution, finally centrifuging, taking supernate and transferring the supernate into a clean centrifugal tube to obtain aminated monolayer PtS 2 And (4) quantum dots.
In the step (2), before discharging, the sealed discharge reactor needs to be vacuumized, ammonia gas is introduced, plasma reaction parameters are set to keep the pressure at-5 kpa-15 kpa, and the gray and black PtS is subjected to different time and power 2 The solid is processed.
In the step (2), setting plasma reaction parameters as electric power of 50-200W and time of 5min-1 h; the treatment time of introducing ammonia gas is 10-60min, and the gas flow rate is 200-400 mL/min. The holding pressure is-5 kpa-15 kpa.
In the step (2), the temperature of vacuum drying is 60-80 ℃.
In step (3), NH 2 -PtS 2 The dosage proportion of the nano-sheets, the isopropanol and the deionized water is 20 mg: 20mL of: 20 mL.
In the step (4), the two-dimensional ultrasonic stripping time is 2-24h, the stripping power is 360W, the cell crushing time is 2-24h, and the crushing power is 360W-450W, and the centrifugal rotating speed is 500-15000 rpm.
Aminated monolayers of PtS prepared according to the invention 2 The preparation method of the quantum dot is applied to photocatalytic hydrogen production as a cocatalyst.
The invention has the beneficial effects that:
the invention provides an aminated monolayer PtS prepared by plasma technology 2 The preparation method of the quantum dot has the advantages that: the method can obtain high-quality aminated single-layer PtS with high efficiency and wide application range 2 The quantum dot material, the preparation process and technology are innovative, and the process is economical, environment-friendly and pollution-free. The invention can prepare aminated monolayer PtS 2 Quantum dots, in addition to aminated monolayer PtS prepared according to the invention 2 The quantum dots can improve the adsorption capacity and reduce the chemical reaction energy barrier, and have excellent catalytic performance and application prospect.
Drawings
FIG. 1 shows Bulk PtS prepared according to the present invention 2 、NH 2 -PtS 2 Nanoplatelets and monolayer NH of example 4 2 -PtS 2 A comparative raman test spectrum of quantum dots.
FIGS. 2(a), (b) and (c) respectively illustrate the preparation of Bulk PtS according to the invention 2 、NH 2 -PtS 2 Nanoplatelets and monolayer NH of example 4 2 -PtS 2 Transmission electron microscope images of quantum dots; (d) (e) (f) are respectively the preparation of Bulk-PtS of the invention 2 、NH 2 -PtS 2 Nanoplatelets and monolayer NH of example 4 2 -PtS 2 Atomic particle display of quantum dotsThe micromirror image.
FIG. 3 is a diagram of the preparation of single-layer NH according to example 4 of the present invention 2 -PtS 2 -QDs/mpg-C 3 N 4 The photocatalytic hydrogen production activity diagram.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
Amination monolayer PtS prepared by plasma technology 2 The preparation method of the quantum dot comprises the following specific steps:
example 1
Firstly, according to the Pt/S atomic ratio of 1:2, evenly mixing platinum powder and sulfur powder, transferring the mixture into a quartz test tube, and sealing the quartz test tube. Placing the sealed quartz tube in a tube furnace, heating at a set temperature of 800 ℃, and obtaining pure gray black PtS after the reaction is finished 2 And (3) solid powder.
50mg of grayish black PtS is weighed 2 Dissolving the solid in 2mL ethanol, uniformly performing ultrasonic treatment, dropping the solution on a quartz plate, drying, placing the quartz plate in a quartz sealed reactor, and generating plasma in a dielectric barrier discharge mode to treat PtS 2 . Before discharging, the quartz reactor needs to be vacuumized for 3min, ammonia gas is introduced for 5min, the pressure is kept at-10 kpa, the plasma reaction parameter is set to be electric power 50W, the reaction time is 10min, and the ammonia gas flow rate is 200 mL/min. Placing the treated sample in a vacuum drying oven at 60 ℃ to obtain NH 2 -PtS 2 -10。
Weighing NH 2 -PtS 2 20mg of-10 solid, adding 20mL of isopropanol and 20mL of deionized water to obtain a mixed solution, performing two-dimensional ultrasonic stripping on the mixed solution for 24h with the power of 360W, performing cell crushing on the mixed solution for 12h with the power of 450W, finally performing centrifugation at 5000rpm, taking supernatant, transferring the supernatant into a clean centrifugal tube, and obtaining small-layer NH 2 -PtS 2 Nanosheets.
The amination Effect of example 1 is that only a small NH layer with a small number of layers is obtained because the plasma treatment time is short 2 -PtS 2 Nanosheets.
Example 2 (variation of the Ammonia plasma treatment time compared to example 1)
Firstly, according to the Pt/S atomic ratio of 1:2, evenly mixing platinum powder and sulfur powder, transferring the mixture into a quartz test tube, and sealing the quartz test tube. Placing the sealed quartz tube in a tube furnace, heating at a set temperature of 800 ℃, and obtaining pure gray black PtS after the reaction is finished 2 And (3) solid powder.
50mg of grayish black PtS is weighed 2 Dissolving the solid in 2mL ethanol, uniformly performing ultrasonic treatment, dropping the solution on a quartz plate, drying, placing the quartz plate in a quartz sealed reactor, and generating plasma in a dielectric barrier discharge mode to treat PtS 2 . Before discharging, the quartz reactor needs to be vacuumized for 3min, ammonia gas is introduced for 5min, the pressure is kept at-10 kpa, the plasma reaction parameter is set to be electric power 50W, the reaction time is 20min, and the ammonia gas flow rate is 200 mL/min. Placing the treated sample in a vacuum drying oven at 60 ℃ to obtain NH 2 -PtS 2 -20。
Weighing NH 2 -PtS 2 20mg of solid 20mg, adding 20mL of isopropanol and 20mL of deionized water to obtain a mixed solution, carrying out two-dimensional ultrasonic stripping on the mixed solution for 24h with the power of 360W, carrying out cell crushing on the mixed solution for 12h with the power of 450W, finally centrifuging at 5000rpm, taking supernatant, transferring the supernatant into a clean centrifugal tube, and obtaining smaller NH with fewer layers 2 -PtS 2 Nanosheets.
The amination effect of example 2 is superior to that of example 1, and mainly shows that the stripping effect is more sufficient, and NH having a less stripped layer is obtained 2 -PtS 2 Nanosheets.
Example 3 (variation of the Ammonia plasma treatment time and discharge Power compared to example 2)
Firstly, according to the Pt/S atomic ratio of 1:2, evenly mixing platinum powder and sulfur powder, transferring the mixture into a quartz test tube, and sealing the quartz test tube. Placing the sealed quartz tube in a tube furnace, heating at a set temperature of 800 ℃, and obtaining pure gray black PtS after the reaction is finished 2 And (3) solid powder.
Weighing50mg Gray Black PtS 2 Dissolving the solid in 2mL ethanol, uniformly performing ultrasonic treatment, dropping the solution on a quartz plate, drying, placing the quartz plate in a quartz sealed reactor, and generating plasma in a dielectric barrier discharge mode to treat PtS 2 . Before discharging, the quartz reactor needs to be vacuumized for 3min, ammonia gas is introduced for 5min, the pressure is kept at-10 kpa, the plasma reaction parameter is set to be 100W, the reaction time is 30min, and the ammonia gas flow rate is 300 mL/min. Placing the treated sample in a vacuum drying oven at 60 ℃ to obtain NH 2 -PtS 2 -30。
Weighing NH 2 -PtS 2 20mg of-30 solid, adding 20mL of isopropanol and 20mL of deionized water to obtain a mixed solution, performing two-dimensional ultrasonic stripping on the mixed solution for 24h with the power of 360W, performing cell crushing on the mixed solution for 12h with the power of 450W, finally performing centrifugation at 5000rpm, taking supernatant, transferring the supernatant into a clean centrifugal tube, and obtaining a lower layer of NH 2 -PtS2 quantum dots.
The amination effect of example 3 is superior to that of examples 1 and 2, mainly in that the stripping time is prolonged, the power is increased, the stripping effect is more sufficient, and less NH layer is obtained 2 -PtS 2 And (4) quantum dots.
Example 4 (time of ammonia plasma treatment, two-dimensional ultrasonic exfoliation and cell disruption was changed as compared with example 3)
Firstly, according to the Pt/S atomic ratio of 1:2, evenly mixing platinum powder and sulfur powder, transferring the mixture into a quartz test tube, and sealing the quartz test tube. Placing the sealed quartz tube in a tube furnace, heating at a set temperature of 800 ℃, and obtaining pure gray black PtS after the reaction is finished 2 And (3) solid powder.
50mg of grayish black PtS is weighed 2 Dissolving the solid in 2mL ethanol, uniformly performing ultrasonic treatment, dropping the solution on a quartz plate, drying, placing the quartz plate in a quartz sealed reactor, and generating plasma in a dielectric barrier discharge mode to treat PtS 2 . Before starting discharging, vacuumizing the quartz reactor for 3min, introducing ammonia gas for 5min, keeping the pressure at-10 kpa, setting the plasma reaction parameters to be electric power of 100W, setting the reaction time to be 60min, and flowing the ammonia gasThe speed is 200 mL/min. Placing the treated sample in a vacuum drying oven at 60 ℃ to obtain NH 2 -PtS 2 -60。
Weighing NH 2 -PtS 2 20mg of solid 60, adding 20mL of isopropanol and 20mL of deionized water to obtain a mixed solution, carrying out two-dimensional ultrasonic stripping on the mixed solution for 36h with the power of 360W, carrying out cell crushing on the mixed solution for 18h with the power of 450W, finally centrifuging at 5000rpm, taking supernatant, transferring the supernatant into a clean centrifugal tube to obtain single-layer NH 2 -PtS 2 And (4) quantum dots.
The amination effect of example 3 is superior to that of examples 1 and 2, mainly in that the stripping time is prolonged, the power is increased, the stripping effect is more sufficient, and a few layers of NH are obtained 2 -PtS 2 And (4) quantum dots.
Raman measurements in FIG. 1 show NH passage 3 Sample NH after plasma treatment, two-dimensional stripping and cell disruption 2 -PtS 2 The lower peak shown by QDs indicates that the samples obtained fewer layers.
TEM and AFM images of FIG. 2 show that we have originally Bulk PtS 2 (a) (d) by passing over NH 3 Plasma treatment to obtain NH 2 -PtS 2 The nano-sheets (b) and (e) have obvious stripping effect, less layer number, and NH is obtained after two-position stripping and cell crushing 2 -PtS 2 The QDs quantum dot has obvious quantum dots with small particle size and small size, and the thinning of the thickness of a sample can be observed corresponding to an AFM picture, which shows that the stripping effect gradually becomes good
Performance testing
Photocatalytic activity measurement method: experiments were performed using an on-line system (Labsolar-6A, PerfectLight, Beijing) to photocatalyze water splitting to produce hydrogen. First, 50mg of the composite photocatalyst was put into a 300mL quartz glass reactor, 100mL of an aqueous solution containing 10mL of Triethanolamine (TEOA) was measured in a graduated cylinder, poured into the reactor and ultrasonically dispersed for 5min to complete photocatalyst dispersion. In the hydrogen production reaction, a 300W Xenon lamp (PLS-SXE300(BF) Perfect Light, Beijing) is used as a Light source, and a cooling circulating water system is controlled within 10 ℃ so as to avoid overhigh temperature for a long time and ensure stable reaction. Every 1 hour, hydrogen production was measured by an on-line gas chromatograph (GC D7900P).
FIG. 3 is a diagram of photocatalytic hydrogen production activity, and the hydrogen production amount can reach 2980.9umol g after 4h of photocatalysis -1 。
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.
Claims (8)
1. Preparation of aminated monolayer PtS by plasma technology 2 The method of quantum dots is characterized by comprising the following steps:
(1) respectively weighing platinum powder and sulfur powder according to a certain proportion, uniformly mixing the platinum powder and the sulfur powder, transferring the mixture into a quartz test tube, sealing the quartz test tube, placing the quartz test tube into a tube furnace, heating the quartz test tube, and obtaining gray black PtS by using a chemical vapor deposition method 2 Opening the tube to take out the solid powder for later use;
(2) weighing the gray black PtS in the step (1) 2 Dissolving the solid in ethanol, ultrasonically homogenizing, dripping on quartz plate, drying, placing the quartz plate in a sealed discharge reactor, and generating plasma in the form of dielectric barrier discharge to treat PtS 2 Vacuum drying after plasma treatment to obtain NH 2 -PtS 2 Nanosheets;
(3) weighing NH in the step (2) 2 -PtS 2 Putting the nanosheet solid into a centrifuge tube, respectively adding the nanosheet solid into a mixed solution of isopropanol and deionized water, and shaking up;
(4) performing two-dimensional ultrasonic stripping on the mixed solution obtained in the step (3), then performing cell crushing on the mixed solution, finally centrifuging, taking supernate and transferring the supernate into a clean centrifugal tube to obtain aminated monolayer PtS 2 And (4) quantum dots.
2. The plasma technique of claim 1, producing an aminated monolayer PtS 2 The method for preparing quantum dots is characterized in that in the step (1), the platinum powder and the sulfur powder are preparedThe dosage ratio is measured according to the atomic ratio of Pt and S of 1:2, and the heating temperature is 800-900 ℃.
3. The plasma technique of claim 1, producing an aminated monolayer PtS 2 The method for quantum dots is characterized in that in the step (2), before discharge, a sealed discharge reactor needs to be vacuumized, ammonia gas is introduced, plasma reaction parameters are set at the pressure of-5 kpa-15 kpa, and gray and black PtS is subjected to different time and power 2 The solid is processed.
4. The plasma technique of claim 1, producing an aminated monolayer PtS 2 The method for preparing the quantum dots is characterized in that in the step (2), the plasma reaction parameters are set to be 50-200W of electric power and 5min-1h of time; the treatment time of introducing ammonia gas is 10-60min, the gas flow rate is 200-400mL/min, and the pressure is kept at-5-15 kpa.
5. The plasma technique of claim 1, producing an aminated monolayer PtS 2 The method for preparing the quantum dots is characterized in that in the step (2), the temperature for vacuum drying is 60-80 ℃.
6. The plasma technique of claim 1, producing an aminated monolayer PtS 2 A method of quantum dot, characterized in that, in the step (3), NH 2 -PtS 2 The dosage proportion of the nano-sheets, the isopropanol and the deionized water is 20 mg: 20mL of: 20 mL.
7. The plasma technique of claim 1, producing an aminated monolayer PtS 2 The method for quantum dots is characterized in that in the step (4), the two-dimensional ultrasonic stripping time is 2-24h, the stripping power is 360W, the cell crushing time is 2-24h, and the crushing power is 360W-450W, and the centrifugal rotation speed is 500-15000 rpm.
8. An aminated monolayer PtS prepared by a process according to any one of claims 1 to 7 2 Quantum dot as cocatalyst in lightApplication to catalytic hydrogen production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210514527.0A CN114950490B (en) | 2022-05-12 | 2022-05-12 | Preparation of amination monolayer PtS by plasma technology 2 Quantum dot method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210514527.0A CN114950490B (en) | 2022-05-12 | 2022-05-12 | Preparation of amination monolayer PtS by plasma technology 2 Quantum dot method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114950490A true CN114950490A (en) | 2022-08-30 |
| CN114950490B CN114950490B (en) | 2023-10-13 |
Family
ID=82981026
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210514527.0A Active CN114950490B (en) | 2022-05-12 | 2022-05-12 | Preparation of amination monolayer PtS by plasma technology 2 Quantum dot method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114950490B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1375459A (en) * | 2001-03-21 | 2002-10-23 | 中国科学院化学研究所 | Prepn. of nano TiO2 powder with high affinity |
| CN108706641A (en) * | 2018-07-23 | 2018-10-26 | 江苏大学 | A kind of preparation method of ultra-thin sulfide nanometer sheet |
| CN109999779A (en) * | 2019-03-12 | 2019-07-12 | 江苏大学 | A kind of In2O3Photochemical catalyst and preparation method and purposes |
| CN109999782A (en) * | 2019-03-11 | 2019-07-12 | 江苏大学 | A kind of photolytic activity defect photochemical catalyst and preparation method and purposes |
| CN110624535A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | Black bismuth tungstate photocatalyst as well as preparation method and application thereof |
-
2022
- 2022-05-12 CN CN202210514527.0A patent/CN114950490B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1375459A (en) * | 2001-03-21 | 2002-10-23 | 中国科学院化学研究所 | Prepn. of nano TiO2 powder with high affinity |
| CN108706641A (en) * | 2018-07-23 | 2018-10-26 | 江苏大学 | A kind of preparation method of ultra-thin sulfide nanometer sheet |
| CN109999782A (en) * | 2019-03-11 | 2019-07-12 | 江苏大学 | A kind of photolytic activity defect photochemical catalyst and preparation method and purposes |
| CN109999779A (en) * | 2019-03-12 | 2019-07-12 | 江苏大学 | A kind of In2O3Photochemical catalyst and preparation method and purposes |
| CN110624535A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | Black bismuth tungstate photocatalyst as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| SHAOZHENG HU ET AL.: ""Improved photocatalytic hydrogen production property over Ni/NiO/N-TiO2-x heterojunction nanocomposite prepared by NH3 plasma treatment"", 《JOURNAL OF POWER SOURCES》, vol. 250, pages 3 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114950490B (en) | 2023-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | High piezo/photocatalytic efficiency of Ag/Bi5O7I nanocomposite using mechanical and solar energy for N2 fixation and methyl orange degradation | |
| Zhang et al. | In situ engineering bi-metallic phospho-nitride bi-functional electrocatalysts for overall water splitting | |
| Pan et al. | MOF-derived C-doped ZnO prepared via a two-step calcination for efficient photocatalysis | |
| He et al. | Enhanced visible light photocatalytic H2 production over Z-scheme g-C3N4 nansheets/WO3 nanorods nanocomposites loaded with Ni (OH) x cocatalysts | |
| CN105271170B (en) | Preparation method of nano carbon and composite material of nano carbon | |
| CN109449002B (en) | Modified Ti3C2TxMaterial, its preparation and use | |
| CN113967475B (en) | Preparation method and application of plasma-induced layered nickel-cobalt double-metal hydroxide photocatalytic material | |
| CN110404567B (en) | Photocatalytic energy conversion material and preparation method and application thereof | |
| CN107651708A (en) | A kind of method that microwave hydrothermal prepares 1T@2H MoS2 | |
| Sun et al. | Plasma-assisted synthesis of pyrrolic-nitrogen doped reduced graphene oxide to enhance supercapacitor performance | |
| CN109225182B (en) | Ultrathin silicon nanosheet photocatalyst and preparation method and application thereof | |
| CN114377708A (en) | Oxygen vacancy-containing bismuthyl carbonate nanosheet and preparation method and application thereof | |
| Liu et al. | A simple hydrothermal method for the preparation of 3D petal-like Ni (OH) 2/g-C3N4/RGO composite with good supercapacitor performance | |
| Wang et al. | Porous WO3 monolith-based photoanodes for high-efficient photoelectrochemical water splitting | |
| Wang et al. | In-situ hydrothermal synthesized γ-Al2O3/Og-C3N4 heterojunctions with enhanced visible-light photocatalytic activity in water splitting for hydrogen | |
| Yang et al. | Oxygen-doped and nitrogen vacancy co-modified carbon nitride for the efficient visible light photocatalytic hydrogen evolution | |
| Zheng et al. | Electron-assisted synthesis of gC 3 N 4/MoS 2 composite with dual defects for enhanced visible-light-driven photocatalysis | |
| Ma et al. | Plasma engraved Bi2MoO6 nanosheet arrays towards high performance supercapacitor and oxygen evolution reaction | |
| Liang et al. | Modulating Charge Separation of Oxygen‐Doped Boron Nitride with Isolated Co Atoms for Enhancing CO2‐to‐CO Photoreduction | |
| Wang et al. | Ion-irradiation of catalyst and electrode materials for water electrolysis/photoelectrolysis cells, rechargeable batteries, and supercapacitors | |
| Li et al. | Graphdiyne (g‐CnH2n− 2)‐supported organic–inorganic composites with zinc cadmium sulfide for photocatalytic hydrogen evolution | |
| Wang et al. | Sp-nitrogen and γ-ray modulating multiply γ-graphyne for anchoring Pt nanoparticles to boost oxygen reduction activity and stability | |
| CN114950490A (en) | Preparation of aminated monolayer PtS by plasma technology 2 Method for quantum dots | |
| Li et al. | SnNb 2 O 6/NiCo-LDH Z-scheme heterojunction with regulated oxygen vacancies obtained by engineering the crystallinity for efficient and renewable photocatalytic H 2 evolution | |
| CN105355839B (en) | Golden combination electrode of a kind of graphene and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |