CN105854901A - Preparation method of molybdenum trioxide and molybdenum disulfide composite material - Google Patents
Preparation method of molybdenum trioxide and molybdenum disulfide composite material Download PDFInfo
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- CN105854901A CN105854901A CN201610252480.XA CN201610252480A CN105854901A CN 105854901 A CN105854901 A CN 105854901A CN 201610252480 A CN201610252480 A CN 201610252480A CN 105854901 A CN105854901 A CN 105854901A
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 208
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract 7
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title abstract 6
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002135 nanosheet Substances 0.000 claims abstract description 17
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 13
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000005987 sulfurization reaction Methods 0.000 claims abstract description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 76
- 229910052750 molybdenum Inorganic materials 0.000 claims description 76
- 239000011733 molybdenum Substances 0.000 claims description 76
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 230000003115 biocidal effect Effects 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000007669 thermal treatment Methods 0.000 claims description 6
- 239000002023 wood Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000011144 upstream manufacturing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000007792 gaseous phase Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 230000000844 anti-bacterial effect Effects 0.000 description 10
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 229940088710 antibiotic agent Drugs 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000005515 coenzyme Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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
- 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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Dentistry (AREA)
- Health & Medical Sciences (AREA)
- Plant Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Inorganic Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a molybdenum trioxide and molybdenum disulfide composite material. The preparation method comprises the following steps of selecting a substrate sheet, cleaning the selected substrate sheet, and preparing a molybdenum trioxide nanosheet by using molybdenum trioxide powder as a growth source and using the cleanly cleaned substrate sheet as the basis by a physical vapor deposition method to obtain the molybdenum trioxide nanosheet; preparing the molybdenum trioxide and molybdenum disulfide composite material by using the obtained molybdenum trioxide nanosheet as a substrate sheet and using powdered sulfur as a sulfur source by a chemical vapor deposition method through high-temperature sulfuration, and obtaining the molybdenum trioxide and molybdenum disulfide composite material. The preparation method of the molybdenum trioxide and molybdenum disulfide composite material is simple, and the implementation is easy. The prepared molybdenum trioxide and molybdenum disulfide composite material can realize photocatalysis response in a visible region, so that the utilization rate of sunlight is greatly improved. The two kinds of materials can be matched, and the effective separation of a photo electron cavity can be realized, so that the composite material shows higher photocatalytic efficiency.
Description
Technical field
The present invention relates to photocatalysis antibacterial material technical field, be more particularly to a kind of molybdenum trioxide
Preparation method with molybdenum bisuphide composite.
Background technology
In medical health field, antibacterial infect the disease caused the most universal.Therefore suppress
Bacterial growth is the most necessary for health.In in the past few decades, antibiotic is
Antibacterial through being widely used for, but antibacterial is easy to antibiotic generation antibody, and antibiotic
It is difficult to apply in biomedical devices.Therefore prepare one layer of antibacterial film pair at medical apparatus surface
It is very important in bacteria growing inhibiting.
Semi-conducting material is the catalysis material that a class application is universal, is applied in life by people
Various aspects, such as fields such as degradable organic pollutant, photolysis water hydrogens.In recent years, science
Family finds to utilize its photocatalysis property, and semi-conducting material can be as the effective anti-biotic material of one.
Wide-band-gap semiconductor material, under the irradiation of ultraviolet light, can produce photo-generate electron-hole pair.These
Light induced electron, hole migration to material surface can generate with the water in air, oxygen reaction and live
Property oxygen.Active oxygen can be with the coenzyme of oxidizing bacteria, and cell membrane the most directly destroys the DNA of antibacterial,
It is finally reached the purpose of sterilization.Molybdenum trioxide is a kind of typical wide bandgap semiconductor, urges at light
Change field has more research.But molybdenum trioxide only has response in ultraviolet light range, and
Ultraviolet light only accounts for about 5% in sunlight, and photohole electronics is to instability, is easily combined,
Photocatalysis efficiency is relatively low.For improving the utilization rate to sunlight and photocatalysis efficiency, to three oxidations
Modifying by more carrying out about many concerns of molybdenum.
Summary of the invention
(1) to solve the technical problem that
The technical problem to be solved in the present invention is how to improve utilization rate and the photocatalysis of sunlight
Efficiency, produces stable electron hole pair, effectively kills antibacterial, and provide a kind of three oxidations
Molybdenum and the preparation method of molybdenum bisuphide composite photocatalyst anti-biotic material.
(2) technical scheme
In order to solve above-mentioned technical problem, the invention provides a kind of molybdenum trioxide and molybdenum bisuphide
The preparation method of composite photocatalyst anti-biotic material (raw materials used the most commercial obtain), this preparation method
Including: preparing molybdenum trioxide nanosheet, gained molybdenum trioxide nanosheet thickness is 100～500nm；
The molybdenum trioxide nanosheet surface sulfide that will obtain, obtains molybdenum trioxide and molybdenum bisuphide composite wood
Material, described thickness of composite material is 100～500nm.
Preferably, this preparation method comprises the following steps that
Step one: choose substrate sheet, its a size of 0.5-2cm × 0.5-2cm, respectively with acetone,
The substrate sheet that second alcohol and water ultrasonic cleaning is chosen, with molybdenum trioxide powder as growth source, utilizes thing
The method of physical vapor deposition, prepares molybdenum trioxide nanosheet based on the substrate sheet cleaned up,
Its preparation condition is: vacuum 10-100Pa, Heating Zone Temperature 700～800 DEG C, substrate section
Temperature 400-700 DEG C, carrying gas is nitrogen or argon, and its flow is 40-80 ml/min,
Response time, 1-10 divided；Then naturally cool to room temperature, obtain molybdenum trioxide nanosheet；
Step 2: the molybdenum trioxide nanosheet obtained using step one as substrate, using sulfur powder as
Sulfur source, utilizes that chemical vapour deposition technique is high temperature vulcanized prepares molybdenum trioxide and molybdenum bisuphide composite wood
Material, its reaction condition is: Heating Zone Temperature is 400～800 DEG C, and sulfur source region temperature is 200～400 DEG C,
Carrying gas is nitrogen or argon, and its flow is 10-60 ml/min, and cure time 5-30 divides；
Then naturally cool to room temperature, obtain molybdenum trioxide and molybdenum bisuphide composite.
Preferably, described substrate sheet is silicon chip, piezoid or aluminium sesquioxide sheet, described
Substrate sheet a size of 1cm × 1cm.
Preferably, in step one, described physical vapour deposition (PVD) is to enter in vacuum tube furnace
OK, by molybdenum trioxide powder as the thermal treatment zone, center of vacuum tube furnace, described substrate is put
In tube furnace airflow downstream low-temperature space.
Preferably, in step 2, described chemical gaseous phase deposition is to enter in vacuum tube furnace
OK, described sulfur powder is placed in air-flow upstream low-temperature space, the molybdenum trioxide that will obtain in step one
Nanometer sheet is placed in the thermal treatment zone, vacuum tube furnace center.
Preferably, in step one, its reaction condition is: vacuum 50Pa, Heating Zone Temperature
785 DEG C, substrate section temperature 550 DEG C, carrying gas is nitrogen, and its flow is 60 ml/min,
Response time 5 points.
Preferably, in step 2, its reaction condition is: Heating Zone Temperature is 600 DEG C, sulfur source
District's temperature is 300 DEG C, and carrying gas is nitrogen, and its flow is 20 ml/min, cure time 10
Point.
Present invention also offers described molybdenum trioxide and molybdenum bisuphide composite photocatalyst anti-biotic material
Molybdenum trioxide prepared by preparation method and molybdenum bisuphide composite.
Present invention also offers described molybdenum trioxide and the purposes of molybdenum bisuphide composite, by institute
The molybdenum trioxide stated and molybdenum bisuphide composite are placed under the illumination of visible ray and irradiate 5-15 minute,
Antibiotic rate reaches more than 99%.
(3) beneficial effect
The molybdenum trioxide of the present invention and the preparation method letter of molybdenum bisuphide composite photocatalyst anti-biotic material
Single easy.Molybdenum trioxide and molybdenum bisuphide composite prepared by the present invention may be implemented in visible ray
The photocatalysis response in region, substantially increases the utilization rate of sunlight.Simultaneously between bi-material
Can mate by band, it is possible to achieve efficiently separating of photo-generate electron-hole, thus composite material exhibits goes out
Higher photocatalysis efficiency.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below
The accompanying drawing used required in embodiment or description of the prior art will be briefly described, aobvious and
Easily insight, the accompanying drawing in describing below is only some embodiments of the present invention, for this area
From the point of view of those of ordinary skill, on the premise of not paying creative work, it is also possible to according to these
Accompanying drawing obtains other accompanying drawing.
Fig. 1 is the SEM figure of molybdenum trioxide prepared by the present invention；
Fig. 2 is the SEM figure of the molybdenum trioxide prepared of the present invention and molybdenum bisuphide composite；
Fig. 3 is the molybdenum trioxide prepared of the present invention and the X-ray diffraction of molybdenum bisuphide composite
Figure；
Fig. 4 is that the EDS of the standby molybdenum trioxide of the present invention and molybdenum bisuphide composite can spectrogram.
Detailed description of the invention
With embodiment, embodiments of the present invention are described in further detail below in conjunction with the accompanying drawings.
Following example are used for illustrating the present invention, but can not be used for limiting the scope of the present invention.
Embodiment 1
(1) take length 1cm, the silicon chip of width 1cm, successively acetone, dehydrated alcohol and
Ultrasonic cleaning in ultra-pure water, the substrate clean to obtain surface；
(2) will be equipped with the corundum boat of 1g molybdenum trioxide powder to be placed in the center of vacuum tube furnace and add
Hot-zone (air-flow upstream), clean silicon chip is placed in tube furnace low-temperature epitaxy district (airflow downstream),
During growth, substrate temperature is about 550 DEG C.Evacuation is to remove the sky in vacuum tube furnace boiler tube
Gas, holding overpressure is 100Pa, and under the nitrogen flow of 60sccm, the thermal treatment zone is extremely
785 DEG C, growth time is 5min.It is then turned off heating and naturally cools to room temperature, obtain three oxygen
Change molybdenum nanometer sheet.
(3) the corundum boat that will be equipped with 0.5g sulfur powder is placed in vacuum tube furnace air-flow upstream low temperature
District, is placed in the thermal treatment zone, vacuum tube furnace center by the molybdenum trioxide nanosheet of preparation in (2).Take out
Vacuum removes inner air tube.Then passing to nitrogen to vacuum tube furnace stove overpressure is normal pressure.
Under the nitrogen flow of 20sccm, sulfur powder temperature is 300 DEG C, and center Heating Zone Temperature is
600 DEG C, jointly keep 10min.It is then turned off heating, naturally cools to room temperature, obtain three
Molybdenum oxide and molybdenum bisuphide composite.
Molybdenum trioxide and the structural characterization of molybdenum bisuphide composite:
The molybdenum trioxide nanosheet that embodiment 1 is obtained and molybdenum trioxide and molybdenum bisuphide composite wood
Material is scanned Electronic Speculum (SEM) observation, and result is as shown in Figure 1 and Figure 2；Three oxidation in Fig. 1
Molybdenum nanometer sheet thickness about 500nm, smooth surface is smooth；In Fig. 2, molybdenum trioxide and molybdenum bisuphide are multiple
Laminate into size is front close with unvulcanized, but rough surface, there is a lot of fold.
Fig. 3 is that the X-ray of the molybdenum trioxide that obtains of embodiment 1 and molybdenum bisuphide composite is spread out
Penetrate figure.From figure 3, it can be seen that the molybdenum trioxide prepared and molybdenum bisuphide composite
Characteristic diffraction peak include molybdenum trioxide (110), (040), (211) and molybdenum bisuphide (002),
(100) characteristic diffraction peak, shows to be successfully prepared molybdenum trioxide and molybdenum bisuphide composite wood
Material；
Fig. 4 is the molybdenum trioxide that obtains of embodiment 1 and the EDS power spectrum of molybdenum bisuphide composite
Figure.From fig. 4, it can be seen that molybdenum (Mo), oxygen (O) and the existence of sulfur (S) three kinds of elements,
And signal intensity is the highest, illustrate that molybdenum trioxide and molybdenum bisuphide composite have three of the above unit
The existence of element.
Embodiment 2
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being to prepare molybdenum trioxide micron film, the temperature of central area is adjusted to 750 DEG C.Products therefrom
Carry out all kinds of signs in embodiment 1, find molybdenum trioxide and the molybdenum bisuphide composite wood of preparation
Expecting less relative to the amount of composite material in embodiment 1, size is the least.Remaining feature is basic
Identical.
Embodiment 3
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being to prepare molybdenum trioxide micron film, the temperature of central area is adjusted to 800 DEG C.Products therefrom
Carry out all kinds of signs in embodiment 1, find that the composite of preparation is relative in embodiment 1
Molybdenum trioxide and molybdenum bisuphide quantity of material more, size is relatively big, but and heterogeneity.Remaining is special
Levy essentially identical.
Embodiment 4
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being and prepare molybdenum trioxide micron film, growth time is adjusted to 10min.Products therefrom carries out reality
Execute all kinds of signs in example 1, find that the composite of preparation is relative to three oxygen in embodiment 1
Changing molybdenum and molybdenum bisuphide quantity of material is more, size is the biggest.Remaining feature is essentially identical.
Embodiment 5
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being and prepare molybdenum trioxide micron film, growth time is adjusted to 30min.Products therefrom carries out reality
Execute the various signs in example 1, find that the composite of preparation is relative to three oxygen in embodiment 1
Change molybdenum and molybdenum bisuphide scantling is much larger, and size heterogeneity, the amount of growth is also the most very
Many.Remaining feature is essentially identical.
Embodiment 6
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being to prepare molybdenum trioxide micron film, substrate temperature is adjusted to 500 DEG C.Products therefrom carries out reality
Execute all kinds of signs in example 1, find that the composite of preparation is relative to three oxygen in embodiment 1
Changing molybdenum and molybdenum bisuphide quantity of material is greatly reduced, size diminishes, pattern heterogeneity, and material exists
Substrate surface distribution is the most sparse.Remaining feature is essentially identical.
Embodiment 7
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
When being to prepare molybdenum trioxide micron film, substrate temperature is adjusted to 650 DEG C.Products therefrom carries out reality
Execute all kinds of signs in example 1, find that the composite of preparation is relative to three oxygen in embodiment 1
Changing molybdenum and molybdenum bisuphide quantity of material is more, size is big much larger than the material obtained in embodiment 1
Little.Remaining feature is essentially identical.
Embodiment 8
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
Be sulfuration molybdenum trioxide micron film when preparing molybdenum trioxide/molybdenum bisuphide composite by the temperature in sulfur source
Degree is adjusted to 200 DEG C.Products therefrom carries out all kinds of signs in embodiment 1, finds preparation
In composite, molybdenum trioxide ratio is higher, relative to the molybdenum trioxide in embodiment 1 and two sulfur
Changing Mo surface more smooth, crystallinity is the best.Remaining feature is essentially identical.
Embodiment 9
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
Be sulfuration molybdenum trioxide micron film when preparing molybdenum trioxide/molybdenum bisuphide composite by the temperature in sulfur source
Degree is adjusted to 400 DEG C.Products therefrom carries out all kinds of signs in embodiment 1, finds preparation
The ratio of composite molybdenum bisuphide is higher, relative to the molybdenum trioxide in embodiment 1 and two sulfur
Changing Mo surface more coarse, crystallinity is worse.Remaining feature is essentially identical.
Embodiment 10
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
It is to vulcanize center heating when molybdenum trioxide micron film prepares molybdenum trioxide and molybdenum bisuphide composite
District's temperature is adjusted to 400 DEG C.Products therefrom carries out all kinds of signs in embodiment 1, finds system
The ratio of standby composite molybdenum trioxide is higher, relative to the molybdenum trioxide in embodiment 1 and
Molybdenum bisuphide material surface is more smooth, and crystallinity is more preferable.Remaining feature is essentially identical.
Embodiment 11
Molybdenum trioxide and molybdenum bisuphide composite is prepared according to the method for embodiment 1, different
It is to vulcanize center heating when molybdenum trioxide micron film prepares molybdenum trioxide and molybdenum bisuphide composite
District's temperature is adjusted to 800 DEG C.Products therefrom carries out all kinds of signs in embodiment 1, finds system
In standby composite, molybdenum bisuphide ratio is higher, relative to the molybdenum trioxide in embodiment 1 and
Molybdenum bisuphide material surface is the most coarse, and crystallinity is worse.Remaining feature is essentially identical.
Test example 1
Performance test:
The molybdenum trioxide and the molybdenum bisuphide composite that embodiment 1 are obtained carry out photocatalysis antibacterial
Performance test:
The photocatalysis antibacterial activity of composite is detected with colony counting method.To cultivate with LB
The staphylococcus aureus that liquid is cultivated overnight, is then diluted to the suspension of 108CFU/ml, takes
80 μ l drop in composite material surface.Xe lamp is light source, add the optical filter of 400-700nm with
Ensureing that light source is visible ray, optical power density is 1W/cm2, illumination contains germy substrate 10
Min, result shows that antimicrobial efficiency is up to more than 99%.It is not added with sample illumination 10min and sample-adding
Two experimental results of product not illumination show, bacterial number and untreated number of bacteria phase
Closely, illustrate that experiment illumination condition used and composite itself are less on bacterial growth impact.Right
Showing under light illumination than experiment, composite has obvious lethal effect to antibacterial, and three oxygen are described
Change molybdenum and molybdenum bisuphide composite has good visible light catalytic anti-microbial property.
Embodiment of above is merely to illustrate the present invention, rather than limitation of the present invention.Although ginseng
Being described in detail the present invention according to embodiment, those of ordinary skill in the art should manage
Solve, technical scheme is carried out various combination, amendment or equivalent, does not takes off
From the spirit and scope of technical solution of the present invention, all should contain in scope of the presently claimed invention
In the middle of.
Claims (9)
1. a molybdenum trioxide and the preparation method of molybdenum bisuphide composite, it is characterised in that
This preparation method includes: prepare molybdenum trioxide nanosheet, and gained molybdenum trioxide nanosheet thickness is
100～500nm；The molybdenum trioxide nanosheet surface sulfide that will obtain, obtains molybdenum trioxide and two
Molybdenum sulfide composite, described thickness of composite material is 100～500nm.
Molybdenum trioxide the most according to claim 1 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that this preparation method comprises the following steps that
Step one: choose substrate sheet, its a size of 0.5-2cm × 0.5-2cm, respectively with acetone,
The substrate sheet that second alcohol and water ultrasonic cleaning is chosen, with molybdenum trioxide powder as growth source, utilizes thing
The method of physical vapor deposition, prepares molybdenum trioxide nanosheet based on the substrate sheet cleaned up,
Its preparation condition is: vacuum 10-100Pa, Heating Zone Temperature 700～800 DEG C, substrate section
Temperature 400-700 DEG C, carrying gas is nitrogen or argon, and its flow is 40-80 ml/min,
Response time, 1-10 divided；Then naturally cool to room temperature, obtain molybdenum trioxide nanosheet；
Step 2: the molybdenum trioxide nanosheet obtained using step one as substrate, using sulfur powder as
Sulfur source, utilizes that chemical vapour deposition technique is high temperature vulcanized prepares molybdenum trioxide and molybdenum bisuphide composite wood
Material, its reaction condition is: Heating Zone Temperature is 400～800 DEG C, and sulfur source region temperature is 200～400 DEG C,
Carrying gas is nitrogen or argon, and its flow is 10-60 ml/min, and cure time 5-30 divides；
Then naturally cool to room temperature, obtain molybdenum trioxide and molybdenum bisuphide composite.
Molybdenum trioxide the most according to claim 2 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that described substrate sheet is silicon chip, piezoid or aluminium sesquioxide sheet, institute
The substrate sheet stated a size of 1cm × 1cm.
Molybdenum trioxide the most according to claim 2 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that in step one, described physical vapour deposition (PVD) is at vacuum tube furnace
In carry out, by molybdenum trioxide powder as the thermal treatment zone, center of vacuum tube furnace, by described base
The end, is placed in tube furnace airflow downstream low-temperature space.
Molybdenum trioxide the most according to claim 2 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that in step 2, described chemical gaseous phase deposition is at vacuum tube furnace
In carry out, described sulfur powder is placed in air-flow upstream low-temperature space, three oxygen that will obtain in step one
Change molybdenum nanometer sheet and be placed in the thermal treatment zone, vacuum tube furnace center.
Molybdenum trioxide the most according to claim 2 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that in step one, its reaction condition is: vacuum 50Pa, heating
District's temperature 785 DEG C, substrate section temperature 550 DEG C, carrying gas is nitrogen, and its flow is 60 millis
Liter/min, the response time 5 points.
Molybdenum trioxide the most according to claim 2 and the preparation side of molybdenum bisuphide composite
Method, it is characterised in that in step 2, its reaction condition is: Heating Zone Temperature is 600 DEG C,
Sulfur source region temperature is 300 DEG C, and carrying gas is nitrogen, and its flow is 20 ml/min, sulfuration
Time 10 points.
8. the molybdenum trioxide described in claim 1-7 and the preparation method of molybdenum bisuphide composite
Prepared molybdenum trioxide/molybdenum bisuphide composite.
9. the molybdenum trioxide described in claim 8 and the purposes of molybdenum bisuphide composite, it is special
Levy and be, described molybdenum trioxide/molybdenum bisuphide composite is placed under the illumination of visible ray photograph
Penetrating 5-15 minute, antibiotic rate reaches more than 99%.
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| CN108341431A (en) * | 2018-01-31 | 2018-07-31 | 天津理工大学 | A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap |
| CN108636426A (en) * | 2018-03-22 | 2018-10-12 | 西北工业大学 | Three-dimensional order is orientated molybdenum disulfide/graphene high-efficiency photocatalysis hydrogen production composite nano materials and preparation method |
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| CN109399953B (en) * | 2018-11-05 | 2021-07-27 | 西北工业大学深圳研究院 | Controllable light absorption type graphene molybdenum disulfide based dimming ecological glass and preparation method thereof |
| CN109399954B (en) * | 2018-11-05 | 2021-12-07 | 西北工业大学深圳研究院 | Gap-controllable molybdenum disulfide-based dimming glass and electrochemical preparation method |
| CN110681400A (en) * | 2019-09-30 | 2020-01-14 | 内江师范学院 | H-molybdenum trioxide/bimetallic sulfide composite material, preparation method and application |
| CN110681400B (en) * | 2019-09-30 | 2022-06-07 | 内江师范学院 | H-molybdenum trioxide/bimetal sulfide composite material, preparation method and application |
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