CN108893974A - One type petal molybdenum disulfide film and its preparation method and application - Google Patents
One type petal molybdenum disulfide film and its preparation method and application Download PDFInfo
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- CN108893974A CN108893974A CN201810581654.6A CN201810581654A CN108893974A CN 108893974 A CN108893974 A CN 108893974A CN 201810581654 A CN201810581654 A CN 201810581654A CN 108893974 A CN108893974 A CN 108893974A
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- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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Abstract
The present invention provides the preparation methods of a type petal molybdenum disulfide film, belong to function nano Material Field.Substrate of the present invention using cotton as molybdenum disulfide film, reduces cost, provides stable support, and cotton high temperature resistant is able to maintain complete fibre structure in hydro-thermal reaction, and gas permeability provides good gas-permeable channels for steam；Using class petal molybdenum disulfide as optical-thermal conversion material, as a type grapheme material, has the advantages that large specific surface area, there is high light absorption in entire solar spectrum, can be converted light into rapidly under light illumination as heat, realize efficient solar steam aggregation, by free of contamination hydro-thermal reaction can a step prepare photothermal conversion film, simple process, easy large area production.Embodiment statistics indicate that, the steam raising rate of class petal molybdenum disulfide film produced by the present invention is up to 1.3kgm‑2·h‑1。
Description
Technical field
The present invention relates to function nano field of material technology more particularly to a type petal molybdenum disulfide film and its preparations
Methods and applications.
Background technique
In 21 century, the shortage of drinking water has become one of most common challenge of facing mankind, with the increasing of population
Long and industry fast development, this problem are just becoming more and more deep-rooted.Recently, solar seawater desalination, as one kind
The technology of low-cost and pollution-less, it has also become focus concerned by people.Cleaning is generated from seawater and industrial wastewater using solar energy
Water is a very promising technology for solving shortage of water resources.For practical application, maximally utilising solar energy is
One necessary technology.Due to a large amount of heat loss, traditional desalination with Solar Energy is infeasible.Utilize photo-thermal base
The sun vaporization method that counterdie carries out local heating is considered as most efficient method in recent years.
The material for the conversion of photo-thermal steam includes gold, the noble metal nanos such as silver fluid and their macroscopic view assembling material at first
Material, but the stability of expensive price and essence easy to reunite and assembled material fragility limits their practical application.Carbon
Nano material is ground, but there are still hardly possiblies extensively because of low cost, excellent light absorption and big specific surface area by researcher
The problem of dispersion, poor air permeability.
Summary of the invention
In consideration of it, the purpose of the present invention is to provide type petal molybdenum disulfide films and its preparation method and application.
Class petal molybdenum disulfide film produced by the present invention easily disperses, and using cotton as substrate, improves the gas permeability of film.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The preparation method of one type petal molybdenum disulfide film, includes the following steps：
(1) dry after impregnating desized cotton in seed solution, the cotton of deposition nucleus is obtained, in the seed solution
Including molybdenum salt and reducing agent；
(2) by the step (1) it is obtained deposition nucleus cotton be immersed in growth solution occur molybdenum disulfide it is spontaneous
Long reaction obtains class petal molybdenum disulfide film, includes molybdenum salt and reducing agent in the growth solution；
Reducing agent in the seed solution and growth solution independently includes in thiocarbamide, sodium thiosulfate and vulcanized sodium
It is one or more；Molybdenum salt and the respective concentration of reducing agent are respectively higher than molybdenum salt and reducing agent in seed solution in the growth solution
Concentration.
Preferably, desized cotton is obtained by cotton through desizing treatment in the step (1), and the temperature of the desizing treatment is
90~100 DEG C, the time of the desizing treatment is 6~12h.
Preferably, in the step (1) in seed solution molybdenum salt concentration be 0.005~0.01mol/L, reducing agent it is dense
Degree is 0.01~0.02mol/L.
Preferably, the concentration of molybdenum salt is 0.01~0.1mol/L, the concentration of reducing agent in growth solution in the step (2)
For 0.02~0.2mol/L.
Preferably, molybdenum salt independently includes sodium molybdate, ammonium molybdate, potassium molybdate and molybdenum in the seed solution and growth solution
One of sour magnesium is a variety of.
It preferably, is 180~200 DEG C from the temperature of growth response in the step (2), it is not small from the time of growth response
In 20h.
Preferably, from after growth response, it will be mixed from growth reaction product with Aqueous Solutions of Polyethylene Glycol and hydro-thermal reaction occurs,
Obtain hydrophily class petal molybdenum disulfide film.
Preferably, the temperature of hydro-thermal reaction is 140~180 DEG C, and the time of the hydro-thermal reaction is 1~2h.
The present invention also provides class petal molybdenum disulfide films made from preparation method described in above-mentioned technical proposal, with cotton
For substrate, grow the molybdenum disulfide nano ball for thering is lamella molybdenum disulfide to be formed by stacking in cotton substrate, dense arrangement by piece
The molybdenum disulfide nano ball of layer superposition forms class petal molybdenum disulfide film.
The present invention also provides class petal molybdenum disulfide films described described in above-mentioned technical proposal in optical-thermal conversion material
In application.
The present invention provides the preparation methods of a type petal molybdenum disulfide film, and desized cotton is soaked in seed solution
It is dry after bubble, the cotton of deposition nucleus is obtained, includes molybdenum salt and reducing agent in the seed solution；The cotton cloth impregnated of nucleus will be deposited
Molybdenum disulfide occurs for bubble from growth response in growth solution, obtains class petal molybdenum disulfide film, includes in the growth solution
Molybdenum salt and reducing agent；Reducing agent in the seed solution and growth solution independently includes thiocarbamide, sodium thiosulfate and vulcanization
One of sodium is a variety of；In the growth solution molybdenum salt and the respective concentration of reducing agent be respectively higher than in seed solution molybdenum salt and
The concentration of reducing agent.Substrate of the present invention using cotton as molybdenum disulfide film, reduces cost, provides stable support,
Cotton high temperature resistant, is able to maintain complete fibre structure in hydro-thermal reaction, and gas permeability provides good ventilative logical for steam
Road；It is excellent with easily dispersing as a type grapheme material using class petal molybdenum disulfide as photothermal conversion active material
Point has high light absorption in entire solar spectrum, can be converted light into rapidly under light illumination as heat, realize efficient solar steam
Aggregation.And preparation process is simple, easy large area production.
Further, the present invention uses Aqueous Solutions of Polyethylene Glycol as hydrophilic modifier, has class petal molybdenum disulfide film
There is good hydrophilicity, improve the delivery rate of water in steam accumulation process, effectively increases solar steam aggregation
Rate.Embodiment statistics indicate that, the steam raising rate of class petal molybdenum disulfide film produced by the present invention is up to 1.3kg
m-2·h-1。
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the class petal molybdenum disulfide film synthetic schemes that the hydrophilic cotton of the embodiment of the present invention 1 is substrate；
Fig. 2 is the scanning electron microscope for the class petal molybdenum disulfide film that cotton hydrophilic made from present example 1 is substrate
Figure, Fig. 2 a are 200 times of enlargement ratios, and Fig. 2 b is 2500 times of enlargement ratios, and Fig. 2 c is 10000 times of enlargement ratios, and Fig. 2 d is 40000
Times enlargement ratio；
Fig. 3 is XRD pair of the class petal molybdenum disulfide film that the hydrophilic cotton of the embodiment of the present invention 1 is substrate and pure cotton cloth
Than figure；
Fig. 4 is the Raman map for the class petal molybdenum disulfide film that 1 cotton of the embodiment of the present invention is substrate, and wherein Fig. 4 a is
Hydrophobic cotton is the Raman map of the class petal molybdenum disulfide film of substrate, and Fig. 4 b is the class petal that hydrophilic cotton is substrate
The Raman map of molybdenum disulfide film；
Fig. 5 is the spectral characteristic for the class petal molybdenum disulfide film that cotton hydrophilic made from present example 1 is substrate
Test chart；
Fig. 6 is the light for the class petal molybdenum disulfide film that cotton hydrophobic and hydrophilic made from present example 1 is substrate
Spectral property comparison diagram, wherein Fig. 6 a is that the reflectance spectrum for the class petal molybdenum disulfide film that hydrophobic and hydrophilic cotton is substrate is special
Property comparison diagram, Fig. 6 b be the class petal molybdenum disulfide film that hydrophobic and hydrophilic cotton is substrate transmission spectral characteristic comparison
Figure；
Fig. 7 is the class petal molybdenum disulfide film that cotton hydrophobic and hydrophilic made from present example 1 is substrate, comparison
The quality of steam loss of water and steam rate change curve, hydrophobic and hydrophilic made from Fig. 7 a present example 1 in example 1,2
Cotton is the class petal molybdenum disulfide film of substrate, the quality of steam of water loses steam rate and changes comparison diagram in comparative example 1,2,
Hydrophobic and hydrophilic cotton made from Fig. 7 b present example 1 is the class petal molybdenum disulfide film of substrate, water in comparative example 1,2
Steam rate change comparison diagram；
Fig. 8 is pure water and hydrophilic cotton is class petal molybdenum disulfide film steam rate change under different illumination of substrate
Change comparison diagram；
Fig. 9 is class petal molybdenum disulfide film steam rate variation and steaming under different illumination that hydrophilic cotton is substrate
Vapour efficiency chart；
Figure 10 is pure water and salt water evaporation rate pair with the class petal molybdenum disulfide film that hydrophilic cotton is substrate
Than figure；
Figure 11 is the cycle performance test chart for the class petal molybdenum disulfide film that hydrophilic cotton is substrate.
Specific embodiment
The present invention provides the preparation methods of a type petal molybdenum disulfide film, include the following steps：
(1) dry after impregnating desized cotton in seed solution, the cotton of deposition nucleus is obtained, in the seed solution
Including molybdenum salt and reducing agent；
(2) by the step (1) it is obtained deposition nucleus cotton be immersed in growth solution occur molybdenum disulfide it is spontaneous
Long reaction obtains class petal molybdenum disulfide film, includes molybdenum salt and reducing agent in the growth solution；
Reducing agent in the seed solution and growth solution independently includes in thiocarbamide, sodium thiosulfate and vulcanized sodium
It is one or more；Molybdenum salt and the respective concentration of reducing agent are respectively higher than molybdenum salt and reducing agent in seed solution in the growth solution
Concentration.
Cotton is preferably carried out desizing treatment by the present invention, obtains desized cotton.In the present invention, the temperature of the desizing treatment
Preferably 90~100 DEG C of degree, the time of the desizing treatment is preferably 6~12h.In the present invention, desizing treatment can remove cotton
Part natural impurity on cloth；Remove the slurry on cotton, such as starch, lubricant, softening agent, plasticizer, preservative；Desizing cotton
Cloth does not have the surface protection of slurry, can preferably carry out the growth of molybdenum disulfide.
The present invention does not have any special restriction to the source of the cotton, using weaving well known to those skilled in the art
Cotton made from method or commercial goods.In the present invention, the area of the cotton is preferably 4.5 × 4.5cm2。
In the present invention, the desizing treatment carries out preferably in sodium hydroxide solution, the sodium hydroxide solution it is dense
Spend preferably 3~5gL-1.The present invention does not have special restriction to the dosage of the sodium hydroxide solution, can be totally submerged cotton
?.
The present invention does not have special restriction to the concrete operations of the desizing treatment, and use is well known to those skilled in the art
Desizing treatment mode, specifically, such as immersing cotton in sodium hydroxide solution, 90 DEG C are heated 6~12 hours, then with 90
DEG C deionized water is washed 6~8 hours, and every two hours replaces a water.By 60~80 DEG C of dryings of cotton of processing and store
It is spare in culture dish.
After obtaining desized cotton, the present invention is dry after the desized cotton is immersed in seed solution, and it is brilliant to obtain deposition
The cotton of core, the seed solution include molybdenum salt and reducing agent；Reducing agent in the seed solution includes thiocarbamide, thiosulfuric acid
One of sodium and vulcanized sodium are a variety of.In the present invention, the molybdenum salt independently preferably includes sodium molybdate, ammonium molybdate, molybdic acid
One of potassium and magnesium molybdate are a variety of.When the molybdenum salt is preferably mixture, the present invention is to molybdenum salt each in the mixture
Dosage there is no special restriction, using the mixture of arbitrary proportion.In the present invention, the solvent in the seed solution
Preferably water.
In the present invention, the concentration of molybdenum salt is preferably 0.005~0.01mol/L in the seed solution, reducing agent it is dense
Degree is preferably 0.01~0.02mol/L.In the present invention, seed solution plays the role of a seed crystal nuclei, and desized cotton is saturated with
Seed solution, subsequent from growth response, since the effect of seed crystal nuclei induces deposition of the molybdenum disulfide on desized cotton,
Achieve the purpose that more homoepitaxial.
In the present invention, when in the seed solution reducing agent be mixture when, the present invention in the mixture respectively also
The amount ratio of former agent does not have special restriction, using the mixture of arbitrary proportion.
The present invention does not have special restriction to the dosage of the desized cotton and seed solution, and seed solution can be made complete
Desized cotton is impregnated, specifically such as by 4.5 × 4.5cm2Desized cotton be immersed in the seed solution of 10~20mL.?
In the present invention, the time of the immersion is preferably 2h.
In the present invention, the temperature of the drying is preferably 60~80 DEG C, and the drying time is preferably 5~6h.At this
In invention, the drying is preferably dried in vacuo.
After obtaining the cotton of deposition nucleus, the cotton for depositing nucleus is immersed in growth solution and molybdenum disulfide occurs by the present invention
From growth response, class petal molybdenum disulfide film is obtained, the growth solution includes molybdenum salt and reducing agent；
Reducing agent in the growth solution includes one of thiocarbamide, sodium thiosulfate and vulcanized sodium or a variety of；It is described
The concentration of molybdenum salt and reducing agent is above the concentration of molybdenum salt and reducing agent in seed solution in growth solution.In the present invention, institute
It is preferably 0.04~0.09mol/L that molybdenum salt, which is stated in growth solution, than the concentration difference of molybdenum salt in seed solution, in the growth solution
Molybdenum salt is preferably 0.08~0.18mol/L than the concentration difference of molybdenum salt in seed solution.
In the present invention, the concentration of molybdenum salt is preferably 0.01~0.1mol/L, the concentration of reducing agent in the growth solution
Preferably 0.02~0.2mol/L.In the present invention, the solvent in the growth solution is preferably water.
In the present invention, when in the growth solution reducing agent be mixture when, the present invention in the mixture respectively also
The amount ratio of former agent does not have special restriction, using the mixture of arbitrary proportion.
The present invention does not have special restriction to the cotton of the deposition nucleus and the dosage of growth solution, can make to grow molten
Liquid is completely soaked the cotton of deposition nucleus, specifically such as by 4.5 × 4.5cm2The cotton of deposition nucleus be immersed in 30mL
Growth solution in.In the present invention, the time of the immersion is preferably 2h.
In the present invention, the molybdenum salt independently preferably includes one of sodium molybdate, ammonium molybdate, potassium molybdate and magnesium molybdate
Or it is a variety of.When the molybdenum salt is preferably mixture, the present invention does not have special limit to the dosage of molybdenum salt each in the mixture
It is fixed, using the mixture of arbitrary proportion.
The present invention does not have special restriction to the preparation method of the seed solution and growth solution, using art technology
The preparation method of composition known to personnel, specifically, such as mixing molybdenum salt, reducing agent and water.In the present invention, described
Mixing preferably carries out under agitation, and the stirring is preferably magnetic agitation, and the revolving speed of the stirring is preferably 300~
750r/min, more preferably 400~550r/min, the mixing time are preferably 20~60min, more preferably 30min.
In the present invention, the temperature from growth response is 180~200 DEG C, is not less than from the time of growth response
20h, more preferably 20h.In the present invention, described preferably to be carried out in a kettle from growth response.
During preparation, the growth that starts of class petal molybdenum disulfide is due to amorphous nanometer MOS 2 particle.
From growth reaction process, sulfiding reagent forms the dual role for serving as sulphur donor and reduction, amorphous molybdenum disulfide nano
Particle shape is at being promoted.In certain temperature and time, these nanoparticle aggregations result in spherical molybdenum disulfide cluster.These
Spherical molybdenum disulfide cluster becomes the seed of molybdenum disulfide nano sheet growth, the Van der Waals being present between monolithic molybdenum disulfide
Interaction facilitates molybdenum disulfide nano sheet and changes to three-dimensional petal molybdenum disulfide.
From after growth response, the present invention preferably will from growth reaction system successively be cooled to room temperature, wash, ethanol washing and
Vacuum drying, obtains class petal molybdenum disulfide film.
In the present invention, the cooling is preferably natural cooling.
The present invention does not have special restriction, energy to the dosage of water and ethyl alcohol, washing times in the washing and ethanol washing
Enough remove unreacted raw material.
In the present invention, the vacuum drying temperature is preferably 60~80 DEG C, and the vacuum drying time is preferably 4
~10h, more preferably 5~7h.
In the present invention, from after growth response, it will be mixed from growth reaction product with Aqueous Solutions of Polyethylene Glycol and hydro-thermal occurs
Reaction, obtains hydrophily class petal molybdenum disulfide film.
In the present invention, the temperature of hydro-thermal reaction is preferably 140~180 DEG C, and more preferably 150 DEG C, the hydro-thermal reaction
Time be preferably 1~2h.In the present invention, in hydrothermal reaction process, the hydrophily of class petal molybdenum disulfide film is improved, is made
Polyethylene glycol penetrates into molybdenum disulfide film, and then the hydrophily got well.
In the present invention, the concentration of the Aqueous Solutions of Polyethylene Glycol is preferably 0.08~0.12gmL-1, more preferably
0.1g·mL-1.The present invention does not have special restriction to the dosage from growth reaction product and Aqueous Solutions of Polyethylene Glycol, specifically
, such as by 4.5 × 4.5cm2From growth reaction product be immersed in the Aqueous Solutions of Polyethylene Glycol of 30mL.
After the completion of hydro-thermal reaction, hydro-thermal reaction system is preferably successively cooled to room temperature, washes by the present invention, ethanol washing and
Vacuum drying, obtains hydrophily class petal molybdenum disulfide film.
In the present invention, the cooling is preferably natural cooling.
The present invention does not have special restriction, energy to the dosage of water and ethyl alcohol, washing times in the washing and ethanol washing
Enough remove unreacted raw material.
In the present invention, the vacuum drying temperature is preferably 60~80 DEG C, and the vacuum drying time is preferably 4
~10h, more preferably 5~7h.
The present invention also provides class petal molybdenum disulfide films made from preparation method described in above-mentioned technical proposal, with cotton
For substrate, grow the molybdenum disulfide nano ball for thering is lamella molybdenum disulfide to be formed by stacking in cotton substrate, dense arrangement by piece
The molybdenum disulfide nano ball of layer superposition forms class petal molybdenum disulfide film.
In the present invention, the thickness of the lamella molybdenum disulfide is preferably 1~5nm, more preferably 2~3nm.
The present invention also provides class petal molybdenum disulfide films described described in above-mentioned technical proposal in optical-thermal conversion material
In application.In the present invention, cotton is that the class petal molybdenum disulfide film of substrate has high light absorption, under light illumination can be rapid
It converts light into as heat, realizes efficient solar steam aggregation.
Class petal molybdenum disulfide film provided by the invention and its preparation method and application is carried out below with reference to embodiment
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) desizing treatment of cotton：Firstly, by 4.5 × 4.5cm2Cotton immerses sodium hydroxide (3gL-1) in solution, 90
DEG C heating 12 hours.Then, it is washed 8 hours with 90 DEG C of deionized waters, and every two hours replaces a water.By the cotton of processing
60 DEG C are dried in vacuo 5 hours and are stored in culture dish for use in future.
(2) molybdenum disulfide growing on cotton certainly：Step (1) desized cotton is immersed in 20mL seed solution i.e. two water
2 hours in the mixed liquor of sodium molybdate (0.01M) and thiocarbamide (0.02M), then it is dried in vacuo 5 hours for 60 DEG C.Then, by its with
The mixed liquor of 30mL growth solution, that is, higher concentration Sodium Molybdate Dihydrate (0.05M) and thiocarbamide (0.1M) is put into reaction kettle, and 200
It DEG C pyroreaction 20 hours, is cooled to room temperature to the end of reacting, with water, ethyl alcohol is cleaned several times, is dried in vacuo 5 hours at 60 DEG C.
Obtain the molybdenum disulfide film that hydrophobic cotton is substrate.
(3) cotton is the hydrophilic treated of the molybdenum disulfide film of substrate：Two using cotton as substrate that step (2) is obtained
Vulcanize molybdenum film and 30mL 0.1gmL-1Aqueous Solutions of Polyethylene Glycol (concentration 0.10gmL-1) it is put into reaction kettle, 150 DEG C of water
Thermal response 1 hour.It is cooled to room temperature to the end of reacting, washes with water several times, 60 DEG C are dried in vacuo 5 hours.It obtains hydrophilic
Cotton is the molybdenum disulfide film of substrate.
Fig. 1 is the class petal molybdenum disulfide film synthesis simple process figure that the hydrophilic cotton of the embodiment of the present invention 1 is substrate.
The process includes three steps：1) desizing treatment of cotton, 2) molybdenum disulfide growing on cotton certainly, 3) polyethylene glycol optimization
Process.The class petal molybdenum disulfide film that hydrophilic cotton is substrate can be obtained in the above manner.
Fig. 2 is the scanning electron microscope for the class petal molybdenum disulfide film that cotton hydrophilic made from present example 1 is substrate
Figure, wherein Fig. 2 a is 200 times of enlargement ratios, and Fig. 2 b is 2500 times of enlargement ratios, and Fig. 2 c is 10000 times of enlargement ratios, and Fig. 2 d is
40000 times of enlargement ratios.From Fig. 2 d, it can be seen that the class petal molybdenum disulfide of apparent lamella superposition.
Fig. 3 is XRD pair of the class petal molybdenum disulfide film that the hydrophilic cotton of the embodiment of the present invention 1 is substrate and pure cotton cloth
Than figure.It can clearly be seen that the diffraction maximum of molybdenum disulfide, wherein XRD spectrum does not show the peak of (002) crystal face, can from Fig. 3
There can be the molybdenum disulfide of few layer of class graphene property to generate, there is an apparent peak to appear in 8.6 °, this is related to interlamellar spacing.
Fig. 4 is the Raman map for the class petal molybdenum disulfide film that cotton of the present invention is substrate, and wherein Fig. 4 a is hydrophobic
Cotton is the Raman map of the class petal molybdenum disulfide film of substrate, and Fig. 4 b is the class petal curing that hydrophilic cotton is substrate
The Raman map of molybdenum film.E12g and A1g peak position difference proves that molybdenum disulfide made from present example 1 is three layers of molybdenum disulfide.
Fig. 5 is the spectral characteristic for the class petal molybdenum disulfide film that cotton hydrophilic made from present example 1 is substrate
Test chart, the absorption including the class petal molybdenum disulfide film that hydrophilic cotton is substrate, penetrates, and reflects map.It can be with from Fig. 5
Find out that the class petal molybdenum disulfide film that hydrophilic cotton is substrate has high light absorption.
Fig. 6 is the light for the class petal molybdenum disulfide film that cotton hydrophobic and hydrophilic made from present example 1 is substrate
Spectral property comparison diagram, wherein Fig. 6 a is that the reflectance spectrum for the class petal molybdenum disulfide film that hydrophobic and hydrophilic cotton is substrate is special
Property comparison diagram, Fig. 6 b be the class petal molybdenum disulfide film that hydrophobic and hydrophilic cotton is substrate transmission spectral characteristic comparison
Figure.As can be seen from Figure 6 spectral absorption of the polyethylene glycol optimization process to the class petal molybdenum disulfide film that cotton is substrate
It has little effect.
Embodiment 2
Hydrophilic cotton prepared by embodiment 1 is that the class petal molybdenum disulfide film (being cut into diameter is 35mm) of substrate passes through
The polystyrene foam of dust-free paper package is swum on 25mL pure water, in intensity of illumination 1kWm-2Lower irradiation 1 hour.
Comparative example 1
25mL pure water is in intensity of illumination 1kWm-2Lower irradiation 1 hour.Disengagement area is same as Example 2.
Comparative example 2
Hydrophobic cotton is the class petal molybdenum disulfide film of substrate, in intensity of illumination 1kWm-2Lower irradiation 1 hour.It steams
Fermentation product is same as Example 2.
As shown in Figure 7a, hydrophilic cotton is substrate for the quality of steam loss of water in testing example 2 and comparative example 1,2
Class petal molybdenum disulfide film has maximum mass loss, and 1 hour loss amount is 1.287kgm-2.Testing example 2 and right
The steam rate variation comparison diagram of water is as shown in Figure 7b in ratio 1,2, and steam raising rate is respectively after stablizing：Pure water
0.24kg·m-2·h-1, hydrophobic cotton is the class petal molybdenum disulfide film 1.16kgm of substrate-2·h-1, hydrophilic cotton
For the class petal molybdenum disulfide film 1.3kgm of substrate-2·h-1。
Embodiment 3
By the preparation method of embodiment 1, intensity of illumination in example example 2 is changed to 2,3,4 or 5kWm-2Lower irradiation 1 hour.
Fig. 8 show pure water and hydrophilic cotton is class petal molybdenum disulfide film steam rate variation pair under different illumination of substrate
Than figure.Obviously hydrophilic cotton is that the steam rate of the class petal molybdenum disulfide film of substrate is significantly larger than the evaporation speed of pure water
Rate.Fig. 9 is class petal molybdenum disulfide film that hydrophilic cotton is substrate steam rate variation and steam effect under different illumination
Rate figure.Its evaporation efficiency can reach 90% or so.
Embodiment 4
By the preparation method of embodiment 1, pure water is only become salt water, light application time by the photothermal measurement method of embodiment 2
Increased to 4 hours by 1 hour.Salt water is by pure water 1000mL, sodium chloride 27.2g, magnesium chloride 3.8g, magnesium sulfate 1.7g, calcium sulfate
1.2g, potassium sulfate 0.1g and calcium carbonate 0.1g are mixed.Figure 10 is with the class petal curing that hydrophilic cotton is substrate
The pure water and salt water evaporation rate comparison diagram of molybdenum film show that salt water is thin to the class petal molybdenum disulfide that hydrophilic cotton is substrate
The evaporation rate of film does not influence significantly.Figure 11 is the cyclicity for the class petal molybdenum disulfide film that hydrophilic cotton is substrate
Energy test chart shows no matter all there is stable photo-thermal effect in salt water or pure water.
Embodiment 5
By the preparation step and experimentation of embodiment 1, growth solution concentration is only adjusted to Sodium Molybdate Dihydrate
(0.01M) and thiocarbamide (0.02M).
Hydrophilic cotton made from embodiment 5 is that the class petal molybdenum disulfide film of substrate is real for steam by embodiment 2
It tests, is similarly obtained the comparing result of Fig. 7, only steam rate is stablized in 0.75kgm-2·h-1。
Embodiment 6
By the preparation step and experimentation of embodiment 1, growth solution concentration is only adjusted to Sodium Molybdate Dihydrate
(0.03M) and thiocarbamide (0.06M).
Hydrophilic cotton made from embodiment 6 is that the class petal molybdenum disulfide film of substrate is real for steam by embodiment 2
It tests, is similarly obtained the comparing result of Fig. 7, only steam rate is stablized in 1.15kgm-2·h-1。
Embodiment 7
By the preparation step and experimentation of embodiment 1, growth solution concentration is only adjusted to Sodium Molybdate Dihydrate
(0.07M) and thiocarbamide (0.14M).
Hydrophilic cotton made from embodiment 7 is that the class petal molybdenum disulfide film of substrate is real for steam by embodiment 2
It tests, is similarly obtained the comparing result of Fig. 7, only steam rate is stablized in 1.32kgm-2·h-1。
Embodiment 8
By the preparation step and experimentation of embodiment 1, growth solution concentration is only adjusted to Sodium Molybdate Dihydrate
(0.1M) and thiocarbamide (0.2M).
Hydrophilic cotton made from embodiment 8 is that the class petal molybdenum disulfide film of substrate is real for steam by embodiment 2
It tests, is similarly obtained the comparing result of Fig. 7, only steam rate is stablized in 1.33kgm-2·h-1。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a type petal molybdenum disulfide film, includes the following steps：
(1) dry after impregnating desized cotton in seed solution, the cotton of deposition nucleus is obtained, includes in the seed solution
Molybdenum salt and reducing agent；
(2) cotton of the obtained deposition nucleus of the step (1) growth solution generation molybdenum disulfide is immersed in grow certainly instead
It answers, obtains class petal molybdenum disulfide film, include molybdenum salt and reducing agent in the growth solution；
Reducing agent in the seed solution and growth solution independently includes one of thiocarbamide, sodium thiosulfate and vulcanized sodium
Or it is a variety of；Molybdenum salt and the respective concentration of reducing agent are respectively higher than the dense of molybdenum salt and reducing agent in seed solution in the growth solution
Degree.
2. preparation method according to claim 1, which is characterized in that desized cotton is by cotton through moving back in the step (1)
Slurry handles to obtain, and the temperature of the desizing treatment is 90~100 DEG C, and the time of the desizing treatment is 6~12h.
3. preparation method according to claim 1, which is characterized in that in the step (1) in seed solution molybdenum salt it is dense
Degree is 0.005~0.01mol/L, and the concentration of reducing agent is 0.01~0.02mol/L.
4. preparation method according to claim 1 or 3, which is characterized in that molybdenum salt in growth solution in the step (2)
Concentration is 0.01~0.1mol/L, and the concentration of reducing agent is 0.02~0.2mol/L.
5. preparation method according to claim 1, which is characterized in that molybdenum salt is independent in the seed solution and growth solution
Ground includes one of sodium molybdate, ammonium molybdate, potassium molybdate and magnesium molybdate or a variety of.
6. preparation method according to claim 1, which is characterized in that be from the temperature of growth response in the step (2)
180~200 DEG C, it is not less than 20h from the time of growth response.
7. preparation method according to claim 1, which is characterized in that from after growth response, will from growth reaction product with
Hydro-thermal reaction occurs for Aqueous Solutions of Polyethylene Glycol mixing, obtains hydrophily class petal molybdenum disulfide film.
8. preparation method according to claim 7, which is characterized in that the temperature of hydro-thermal reaction is 140~180 DEG C, described
The time of hydro-thermal reaction is 1~2h.
9. class petal molybdenum disulfide film made from preparation method described in claim 1~8 any one, using cotton as substrate,
In cotton substrate grow there is lamella molybdenum disulfide to be formed by stacking molybdenum disulfide nano ball, dense arrangement by lamella superposition
Molybdenum disulfide nano ball forms class petal molybdenum disulfide film.
10. application of the class petal molybdenum disulfide film as claimed in claim 9 in optical-thermal conversion material.
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