CN107116231A - A kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane - Google Patents
A kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane Download PDFInfo
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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Abstract
The invention discloses a kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, the preparation method of the individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane mainly includes：Gold nano grain self-assembled monolayer, molybdenum disulfide single thin film；Both thin-film materials constitute entirety by Van der Waals force formation individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, and with base material.The present invention makes full use of the Cooperative Excitation of gold nano grain self-assembled monolayer and molybdenum disulfide single thin film in individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane to act on and produces photoelectric properties high-gain, individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite film thickness of preparation is homogeneous controllable, collective's surface plasmon resonance effect of gold nano grain self-assembled monolayer is as exciting pumping, the luminescence generated by light and photoelectric transformation efficiency of molybdenum disulfide single thin film can greatly be strengthened, in following photoelectric device, bio-photon, field-effect transistor, the photoelectric fields such as photo-detector have great advantage.
Description
Technical field
The invention belongs to field of material technology, further relate to a kind of individual layer in technical field of nanometer material preparation from
Assemble the preparation method of gold nano grain/molybdenum disulfide composite membrane.The present invention can be used for the sulphur of individual layer self-assembling of gold nanoparticles/bis-
Change the preparation of molybdenum composite membrane.
Background technology
Molybdenum disulfide, as one of most representational emerging two-dimensional layer material, is another after graphene to enjoy pass
The semi-conducting material of note, its layer is combined with interlayer by weaker Van der Waals force, thus can be stripped into two-dimensional layer nanometer
Material, its physical property has obvious thickness dependence, and with the reduction of the atom number of plies, it is transitioned into directly by indirect band gap
Also there is the enhancing of respective degrees in band gap, luminescence generated by light, photoelectric transformation efficiency, make it in photoelectron, energy stores and field-effect
The various fields such as transistor have a good application prospect.However, single molybdenum disulfide luminescence generated by light and photoelectric transformation efficiency
It is high not enough, the higher demand that current photoelectric field is proposed to its performance can not have been met.At present, molybdenum disulfide light is effectively improved
The method of photoluminescence and photoelectric transformation efficiency is usually that noble metal nanometer material and molybdenum disulfide are carried out into hydridization, because its is efficient
Cooperative Excitation effect can produce photoelectric properties high-gain, and especially most representational gold nano grain is because of its excellent surface etc.
Ion plasmon resonance characteristic and receive and pay close attention to.Under the conditions of controllable growth, uniform spherical gold nano grain in it is each to
The same sex, and gold nano grain can self assembly be single thin film, show more excellent collective's optic response.This seminar is
Granted patent technology " a kind of preparation method of gold nano grain self assembly portable single thin film "（The patent No.：ZL
201510765301.8）In disclose a kind of preparation method of gold nano grain self assembly portable single thin film.The patent skill
Gold nano grain self-assembled monolayer large area prepared by art is continuous, and thickness is homogeneous controllable, and stability is good, can protect for a long time
Deposit, can be transplanted on any substrate, and realize self assembly gold nano grain average grain diameter be 6nm, dimensional discrepancy is about
For 6%, it is adapted to excite pumping using its collective's Plasmon Resonance effect.
Therefore, compared to gold nano particle modification molybdenum disulfide is directly used, the uniform gold nano of particle diameter distribution is passed through
Grain is self-assembly of transplantable gold nano grain single thin film, enables to the compact arranged gold nano grain of large area uniform
Ground deposition is covered on molybdenum disulfide single thin film, by the use of its remarkable collective's surface plasmon resonance effect as exciting
Pumping, strengthens the luminescence generated by light and photoelectric transformation efficiency of molybdenum disulfide single thin film to greatest extent.
Patented technology " a kind of molybdenum disulfide/gold nanorods composite, the preparation method of State Nanometer Science Center's application
And purposes "（Application number 201410815045.4, application publication number CN104525938 A）In disclose a kind of molybdenum disulfide/gold
Nanometer rod composite material, Preparation method and use.This method relies on electrostatic interaction, will in electronegative molybdenum disulfide nano sheet and
It is compound in electropositive gold nanorods, molybdenum disulfide/gold nanorods composite is obtained, gold nanorods refer in 30nm or so
Go out the molybdenum disulfide/gold nanorods composite available for photo-thermal therapy.The patented technology exist weak point be：Gold nano
Rod is monodimension nanometer material, and its intrinsic anisotropy makes the interaction between gold nanorods have directional dependence, therefore
Its Plasmon Resonance effect is relatively worse than smaller szie and in isotropic spherical gold nano grain.
The patented technology of University Of Ji'nan's application be " a kind of nano-particle modified three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide of Au
Preparation method "（Application number 201510418712.X, application publication number CN105152215 A）In disclose a kind of Au nano particles
Modify the preparation method of three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide.The invention is with gold chloride, sodium borohydride, 1B and
The molybdenum disulfide of preparation is raw material, a kind of Au modifications three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide of reaction synthesis at normal temperatures, and
Gained Au modification three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide can be used for the fields such as chemical industry catalysis, photochemical catalyst gas sensor.
The patented technology exist weak point be：The particle diameter heterogeneity of gold nano grain, dimensional discrepancy is larger, and it is classified in three-dimensional
Settled density on structure flower ball-shaped molybdenum disulfide is small and uneven.
" a kind of laser-induced material reproducibility prepares polymorphic gold nano structure to the patented technology of Beijing Institute of Technology's application
Method "（Application number 201610178556.9, application publication number CN105642913 A）In disclose a kind of molybdenum disulfide/gold
The preparation method of nanostructure composite material.The reaction makes it produce reproducibility, leaching with laser pulse induction molybdenum disulfide film
Polymorphic Jenner can be obtained on molybdenum disulfide film surface by entering in the chlorauric acid solution of debita spissitudo and taking out drying process
Rice structure.The patented technology, which exists, to be disadvantageous in that：Obtained gold nano cluster size is larger, is difficult to embody nano material
Small-size effect, the peculiar property such as skin effect, the deposition of gold nano structure is not uniform enough and deposition is relatively low.Employ femtosecond
The equipment such as laser double-pulse generating means, it is with high costs and limit and promote the use of.
The content of the invention
It is an object of the invention to overcome the shortcomings of that above-mentioned prior art is present, overcome gold nanorods large scale and it is each to
The opposite sex, and sunk by the composite that particle diameter heterogeneity, the dimensional discrepancy of gold nano be larger, dispersed and randomness is brought
Product coverage rate is too low, and the problem of deposition position arbitrariness.It is simply single that the present invention provides a kind of easily operated, preparation process
The preparation method of layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, gold nano grain pattern is homogeneous, size uniform and deviation
Small, its self-assembling nanoparticles can obtain efficient collective's Plasmon Resonance effect of two-dimensional nano-film, can give play to more
The good pumping that excites is acted on, and constructed individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite film thickness is homogeneous controllable, has
Fabulous surface plasmon resonance characteristic and opto-electronic conversion performance, can be applied to following photoelectric device, bio-photon and
The fields such as photo-detector.This method has fabulous Scientific Research Potential and application value.
Realizing the thinking of the object of the invention is, the present invention prepares the list of particle size uniformity by the phase method of a step one first
Scattered gold nano grain solution, and using ethylene glycol as phase under face, to gold nano grain on immiscible liquid surface
Self assembly is adjusted, and obtains no substrate limitation and visible, the gold nano grain single thin film freely suspended of naked eyes；Secondly, profit
With chemical vapour deposition technique molybdenum disulfide single thin film is prepared on 300nm thick oxide layer silicon chips；Finally, by gold nano grain list
Layer film carries out mechanical transfer and is coated with molybdenum disulfide single thin film, obtains individual layer self-assembling of gold nanoparticles/curing
Molybdenum composite membrane.
Realize the specific steps of the object of the invention including as follows：
（1）Obtain gold nano grain single thin film：
（1a）Gold nano grain is prepared using the phase method of a step one, the average grain diameter of gold nano grain is 6nm, and dimensional discrepancy is about
6%；
（1b）Phase under face is made using ethylene glycol, volatilize minim organic solvent on immiscible liquid surface, realizes gold nano
The self assembly of grain, obtains transplantable gold nano grain single thin film；
（2）Obtain molybdenum disulfide single thin film：
Grown using chemical vapour deposition technique on base material and obtain molybdenum disulfide single thin film；
（3）Prepare individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane：
Using molybdenum disulfide single thin film and base material to be overall, gold nano grain single thin film is shifted and is coated with to two
The surface of molybdenum sulfide single thin film, obtains individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane.
The present invention has advantages below compared with prior art：
First, the present invention is homogeneous using pattern, and average grain diameter is 6nm, and the spherical gold nano grain that dimensional discrepancy is about 6% is from group
Dress forms transplantable single thin film, and it has continuous large area, homogeneous controllable, the gold nano grain marshalling of thickness, long-range
In order the characteristics of, and molybdenum disulfide single thin film surface is coated with, overcome in national nano science of the prior art
The patented technology " a kind of molybdenum disulfide/gold nanorods composite, Preparation method and use " of heart application（Application number
201410815045.4, application publication number CN104525938 A）Middle gold nanorods size is 30nm, its intrinsic anisotropy
Make the interaction between gold nanorods that there is directional dependence, Plasmon Resonance effect is relatively worse than smaller szie and in each
To this weak point of the spherical gold nano grain of the same sex, and overcome the patented technology of University Of Ji'nan's application in the prior art
" a kind of preparation method of the nano-particle modified three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide of Au "（Application number
201510418712.X, application publication number CN105152215 A）The particle diameter heterogeneity of middle gold nano grain, dimensional discrepancy is larger,
And its settled density on three-dimensional hierarchical structure flower ball-shaped molybdenum disulfide is small and uneven this weak point.
Second, the preparation method for individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane that the present invention is provided, equipment letter
Single, it is easy to operate, preparation process is easy, and molybdenum disulfide single thin film is by the homogeneous continuous gold nano of controllable, large area of thickness
After granular cell layer is film modified, gold nano grain can be more evenly distributed on molybdenum disulfide single thin film, compared to single
Gold nano grain, the single thin film of its self assembly shows more excellent collective's optic response, therefore in gold nano grain
There is extremely strong optical coupled effect between single thin film and molybdenum disulfide single thin film so that individual layer self assembly gold nano
The luminescence generated by light and photoelectric transformation efficiency of grain/molybdenum disulfide composite membrane are greatly enhanced, photoelectric device, bio-photon,
The photoelectric fields such as field-effect transistor, photo-detector and photovoltaic synergy have great advantage.
Brief description of the drawings
Fig. 1 is the schematic diagram of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane in the present invention；
Fig. 2 is technical process figure of the invention.
Embodiment
The present invention will be further described below in conjunction with the accompanying drawings.
Referring to the drawings 1, individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane of the invention includes：Gold nano grain
Single thin film, molybdenum disulfide single thin film；Gold nano grain single thin film is coated with molybdenum disulfide single thin film surface, two kinds
Thin-film material is constructed by Van der Waals force obtains individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, and and base material
Constitute overall.
Referring to the drawings 2, a kind of preparation side for individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane that the present invention is provided
Method, from step, is broadly divided into the preparation of gold nano grain single thin film and molybdenum disulfide single thin film, but the individual layer constructed
The simple addition of self-assembling of gold nanoparticles/molybdenum disulfide composite membrane not the two function, this individual layer self assembly gold nano
Grain/molybdenum disulfide composite membrane shows the optics of uniqueness, electrology characteristic, has both possessed the high luminescence generated by light of molybdenum disulfide single thin film
And photoelectric transformation efficiency, the Plasmon Resonance property of gold nano grain single thin film is also equipped with, while utilizing gold nano
The Plasmon Resonance effect of grain single thin film drastically increases this orderly hybrid nanostructure as pumping is excited
Luminescence generated by light and photoelectric transformation efficiency.Embodiments of the invention are comprised the following steps that.
Step 1, gold nano grain single thin film is obtained.
0.25mmol triphenyl phosphorus chlorine gold is dissolved in 25ml toluene, 1mmol dodecyl mercaptans is added, obtains solution A
Presoma.
2.5mmol monoboranes-tert-butylamine complex compound is dissolved in 15ml toluene, the presoma of solution B is obtained.
At room temperature, the presoma of the presoma of solution A, solution B is respectively placed in into heating in 90-100 DEG C of silicone oil bath to stir
Mix to being completely dissolved, obtain solution A and solution B.
Solution B is rapidly added in solution A dropwise, mixed solution is obtained.
Mixed solution is placed in heating stirring 5min in 100 DEG C of silicone oil baths.
Mixed solution is naturally cooled into room temperature, the stoste of gold nano grain is obtained.
Absolute ethyl alcohol is added in gold nano grain stoste, to the centrifugation of gold nano grain stoste twice, centrifuged twice
Condition is that the absolute ethyl alcohol added for the first time and the gold nano grain stoste centrifuged are to wait to match somebody with somebody specific volume, and centrifugal rotational speed is
3000rpm, a length of 2min during centrifugation；The half of the absolute ethyl alcohol of second of addition absolute ethyl alcohol volume added by for the first time, from
Heart rotating speed is 2000rpm, a length of 2min during centrifugation；Obtain the black precipitate of gold nano grain.
The black precipitate of gold nano grain is dried, then by dry gold nano grain black precipitate dissolving in hexane,
The volume of added hexane is centrifuged the 1/3 of gold nano grain stoste volume, obtains the hexane solution containing gold nano grain.
By the hexane solution containing gold nano grain rotating speed be 5000rpm, when a length of 5min under conditions of centrifuge once, obtain
Average grain diameter to gold nano grain is 6nm, and dimensional discrepancy is about 6%, the oil phase monodisperse gold particle of particle size uniformity
Pure solution.
The 100 pure solution of μ l gold nano grains are measured into test tube, 900 μ l hexanes is added, obtains diluting 10 times of gold
The dilute solution of the pure solution of nano particle.
The gold nano grain dilute solution for diluting 10 times is added in quartz colorimetric utensil, UV, visible light spectrophotometric is used
Measurement examination dilutes maximum absorbance of 10 times of the gold nano grain dilute solution in 300nm-800nm wave-length coverages.
It is 6nm according to the particle diameter of gold nano grain in 10 times of gold nano grain dilute solution is diluted, is obtained through tabling look-up
The absorptivity of gold nano grain is ε=3 × 106 mol-1·L·cm-1。
By Lambert-Beer's law, the concentration C for the gold nano grain dilute solution for obtaining 10 times of dilution is calculated1。
According to C2 =10·C1, the concentration for obtaining the pure solution of gold nano grain is calculated, wherein, C1For 10 times of Jenner of dilution
The concentration of rice grain dilute solution.
8ml ethylene glycol is measured into polytetrafluoroethylene beaker.
It is 0.5 × 10 by 5 μ l granule densities-6 Mol/L gold nano grain solution drops to ethylene glycol surface, covers glass
Piece stands 15-30min, obtains being suspended in the transplantable gold nano grain single thin film on ethylene glycol surface.
Step 2, molybdenum disulfide single thin film is obtained.
The sulfur powder that the molybdenum trioxide powder for being 99.5% by 0.1g purity and 0.3g purity are 99.95% is respectively placed in two
In quartz boat, the quartz boat that will be equipped with molybdenum trioxide powder is placed at the airflow downstream of tube furnace constant temperature zone, equipped with sulfur powder
Quartz boat be placed in air-flow upstream end.Silicon chip layer as substrate is fixed on the quartz boat equipped with molybdenum trioxide down
Side.
Tube furnace is sealed, vacuumizing makes to reach oxygen-free environment in pipe.Then it is continually fed into the High Purity Nitrogen that flow velocity is 100sccm
Gas（99.999%）30min, and air pressure in vacuum drying oven is kept normal pressure.
Change Ventilation Rate to 30sccm, and start to sulphur powder and molybdenum trioxide powder while heating.Make three oxidations
Molybdenum powder rises to 500 DEG C in 30min by room temperature, and 650 DEG C are warming up to by 500 DEG C in 15min.Meanwhile, make in 45min
Sulphur powder is by room temperature to 200 DEG C.
Make sulphur powder and molybdenum trioxide powder respectively at a temperature of 200 DEG C and 650 DEG C while keeping constant temperature 5min, then close
Closing thermal source makes tube furnace Temperature fall, treats that temperature is down to less than 100 DEG C opening tube furnaces.Nitrogen flow rate is maintained at during cooling
30sccm。
Vacuum tube furnace is opened, base material is taken out, there is molybdenum disulfide single thin film on its surface.
Step 3, individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane is prepared.
Using molybdenum disulfide single thin film and base material to be overall, gold nano grain single thin film is shifted and is coated with
To molybdenum disulfide single thin film surface, individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane is obtained.
Claims (5)
1. a kind of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, including gold nano grain self-assembled monolayer, two
Molybdenum sulfide single thin film, it is characterised in that the gold nano grain self-assembled monolayer is coated with molybdenum disulfide single thin film
Surface, two kinds of thin-film materials are constructed by Van der Waals force obtains individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, and with
Base material constitutes overall.
2. a kind of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane according to claim 1, it is characterised in that
The base material uses 300nm thick oxide layer silicon chips.
3. a kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane, comprises the following steps：
（1）Obtain gold nano grain single thin film：
（1a）Gold nano grain is prepared using the phase method of a step one, the average grain diameter of gold nano grain is 6nm, and dimensional discrepancy is about
6%；
（1b）Phase under face is made using ethylene glycol, volatilize minim organic solvent on immiscible liquid surface, realizes gold nano
The self assembly of grain, obtains transplantable gold nano grain single thin film；
（2）Obtain molybdenum disulfide single thin film：
Grown using chemical vapour deposition technique on base material and obtain molybdenum disulfide single thin film；
（3）Prepare individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane：
Using molybdenum disulfide single thin film and base material to be overall, gold nano grain single thin film is shifted and is coated with to two
Molybdenum sulfide single thin film surface, obtains individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane.
4. a kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane according to claim 3, its
It is characterised by, step（1b）Described in gold nano grain single thin film in single nanoparticle unit pattern be spherical, Jenner
The thickness of rice grain single thin film is 6nm.
5. a kind of preparation method of individual layer self-assembling of gold nanoparticles/molybdenum disulfide composite membrane according to claim 3,
Characterized in that, step（2）Described in molybdenum disulfide monolayer film thickness be 6.5.
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