CN109576658A - Dendroid amorphous MoS is prepared based on magnetron sputtering method2The method of nanostructure - Google Patents
Dendroid amorphous MoS is prepared based on magnetron sputtering method2The method of nanostructure Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The present invention relates to photoelectrocatalysimaterial material technical fields, and in particular to one kind prepares dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, with MoS2As target, using quartz plate as substrate, target, substrate are arranged in closed environment, the distance between substrate and target are adjusted to 9~12cm, and the angle of substrate and horizontal plane is adjusted to 0 °~15 °, start to sputter by d.c. sputtering source, sputtering time is 40~90min, obtains dendroid amorphous MoS2Nanostructure.The present invention is by that can effectively reduce the energy of deposited particles under the mutual cooperation of low pressure, low-angle, the slow-speed of revolution, low current, target-substrate distance appropriate and argon flow, make incoming particle it is relatively stable grow into the material with nanostructure, make dendroid amorphous MoS obtained2Nanostructure large specific surface area promotes MoS2The photoelectric properties of catalysis material can be widely used in photocatalytic redox field.
Description
Technical field
The present invention relates to photoelectrocatalysimaterial material technical fields, and in particular to one kind is non-based on magnetron sputtering method preparation dendroid
Brilliant MoS2The method of nanostructure.
Background technique
Since 20th century, with the rapid development of society, the problems such as following some energy shortages, environmental pollution, more comes
Severeer.Conductor photocatalysis material has very big researching value in the solution energy, environmental problem.MoS2Semiconductor material tool
There is the features such as narrow band gap, two-dimensional layered structure, has certain practical value on the fields such as photocatalysis and aerospace industry.With it is common
Molybdenum disulfide is compared, the MoS with nanostructure2Catalysis material has big specific surface area, and can improve light in nano junction
Scattering between structure increases nano material to the sink effect of light, therefore can effectively improve its photocatalysis performance.MoS2Nanometer
Material can pass through hydro-thermal method, template, mechanical stripping method, electrochemical stripping method, solvent-thermal method, hydrodynamic, ball milling
The preparation such as method, Hummer method, steam blow, ultrasonic water bath method, but the preparation process of the above method is relatively complicated, inconvenient big rule
The preparation of mould.
In addition, in the preparation method of existing molybdenum disulfide, one as disclosed in China Patent Publication No. CN103205724A
The preparation method of kind molybdenum disulfide film material, with MoS2Target is raw material, in argon gas and hydrogen sulfide mixed-gas environment, is led to
It crosses magnetron sputtering method and prepares MoS in substrate2Film, molybdenum disulfide film material with a thickness of 0.1-10.0 μm；The invention
Advantage is: by using Ar gas-H in magnetron sputtering technique2S gaseous mixture and substrate heat in-situ annealing mode, it is ensured that MoS2
Film realizes uniform deposition and S/Mo atomic ratio is maintained at 2: 1, and thickness can be effectively increased by increasing sputtering time, improves MoS2
Nano thin-film yield, but molybdenum disulfide material photoelectric properties made from this method are poor.
For this purpose, the present invention provides a kind of dynamic glancing angle deposition technology based on magnetron sputtering technique development, preparation has
The amorphous MoS of dendritic nanostructure2Material effectively raises the photoelectrocatalysis property of material, can be realized large area
The preparation of scale has important application value.
Summary of the invention
It is non-based on magnetron sputtering method preparation dendroid that it is an object of the invention to overcome the deficiencies of the prior art and provide one kind
Brilliant MoS2The method of nanostructure, by low pressure, low-angle, the slow-speed of revolution, low current, target-substrate distance appropriate and argon flow
Cooperate the lower energy that can effectively reduce deposited particles, makes incoming particle is relatively stable to grow into nanostructure
Material makes dendroid amorphous MoS obtained2Nanostructure has good photoelectric properties.
The purpose of the present invention is achieved through the following technical solutions:
One kind preparing dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, with MoS2As target, with stone
Target, substrate are arranged in closed environment as substrate for English piece, and adjustment the distance between substrate and target are 9cm~12cm,
And the angle of substrate and horizontal plane is adjusted to 0 °~15 °, then by closed environment vacuumize process, in closed environment air pressure drop
To 2 × 10-4When, argon gas is passed through into closed environment as sputter gas；Then control closed environment air pressure be 0.15Pa~
0.2Pa starts to sputter by d.c. sputtering source, and sputtering time is 40min~90min, obtains dendroid amorphous MoS2Nano junction
Structure.
Further, the MoS2It is not less than 99.99% MoS using purity2。
Further, the quartz plate is first successively cleaned by ultrasonic in acetone, dehydrated alcohol, deionized water, then
It is dried with nitrogen, is re-used as substrate.
Further, the quartz plate is successively cleaned by ultrasonic that 20min, ultrasound is clear in ethanol solution in acetone soln
It washes 20min, be cleaned by ultrasonic 5min in solution in deionized water.
Further, the substrate spins in sputtering process.
Further, the spin revolving speed of the substrate is 1r/min.
Further, the sputtering current in the d.c. sputtering source is 0.1A.
Further, the flow of the argon gas is 12.5sccm~20sccm.
Further, it is prepared by magnetron sputtering apparatus.
The beneficial effects of the present invention are: proposed by the present invention prepare dendroid amorphous MoS based on magnetron sputtering method2Nano junction
The method of structure, preparation cost is low, and preparation process is simple, and sample repeatability is high, free from environmental pollution, by low pressure, low-angle,
The slow-speed of revolution, low current, target-substrate distance appropriate and argon flow cooperate the lower energy that can effectively reduce deposited particles, make into
Radion is relatively stable to grow into the material with nanostructure, makes dendroid amorphous MoS obtained2Nanostructure specific surface
Product is big, and big specific surface area can provide more active site for photocatalytic process, to effectively promote MoS2Photocatalysis material
The photoelectric properties of material can be widely used in photocatalytic redox field.
Detailed description of the invention
Fig. 1 is dendroid amorphous MoS made from test example 1 of the present invention2100000 times of scanning electron microscopies of nanostructure
Mirror (SEM) photo；
Fig. 2 is dendroid amorphous MoS made from test example 1 of the present invention2100000 times of scanning electron microscopies of nanostructure
Mirror (SEM) cross-section photograph；
Fig. 3 is dendroid amorphous MoS made from test example 1 of the present invention2The ultraviolet-visible light (UV-vis) of nanostructure is inhaled
Receive map；
Fig. 4 is dendroid amorphous MoS made from test example 1 of the present invention2The time current densogram of nanostructure；
Fig. 5 is dendroid amorphous MoS made from test example 1 and test example 2 of the present invention2The I-V diagram of nanostructure is composed.
Fig. 6 is dendroid amorphous MoS of the present invention2The illustraton of model of nanostructure.
Specific embodiment
Technical solution of the present invention, but protection of the invention are described in further detail with attached drawing combined with specific embodiments below
Range is not limited to as described below.
Embodiment
One kind preparing dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, with MoS2As target, with stone
English piece target, substrate is arranged in closed environment as substrate, by the distance between substrate and target adjust to 9cm~
12cm, and the angle of substrate and horizontal plane is adjusted to 0 °~15 °, then by closed environment vacuumize process, in closed environment
Air pressure is down to 2 × 10-4When, argon gas is passed through into closed environment as sputter gas；Then control closed environment air pressure be
0.15Pa~0.2Pa starts to sputter by d.c. sputtering source, and sputtering time is 40min~90min, obtains dendroid amorphous
MoS2Nanostructure.
Specifically, the MoS2It is not less than 99.99% MoS using purity2；The quartz plate is successively in acetone soln
Ultrasonic cleaning 20min, it is cleaned by ultrasonic 20min in ethanol solution, is cleaned by ultrasonic 5min in deionized water solution；The substrate
It spins in sputtering process, spin revolving speed is 1r/min；The sputtering current in the d.c. sputtering source is 0.1A；The stream of the argon gas
Amount is 12.5sccm~20sccm.
Test example 1
The preparation method of this test example the following steps are included:
Step 1: substrate raw material is successively placed on third using the quartz plate of regular shape and electro-conductive glass as substrate raw material
Respectively it is cleaned by ultrasonic 20 minutes in ketone, ethanol solution, is then cleaned by ultrasonic 5 minutes in deionized water again, with is dried with nitrogen
Its surface moisture, it is spare as sample substrate；
Step 2: being 99.99%, diameter 6cm by purity, with a thickness of the MoS of 5mm2Target is mounted on magnetic control sputtering device
No. 2 target position of device, then the quartz plate cleaned up in step 1 and electro-conductive glass are fixed on disk with high temperature gummed tape, it is conductive
Glass reserves the surface area of 5mm × 5mm, while disk being fixed in rotatable base station, and adjustment target-substrate distance is 10cm, circle
The angle of disk plane and horizontal plane is 5 °；
Step 3: closing magnetron sputtering chamber door, mechanical pump is opened, to cavity vacuumize process, when cavity air pressure drops to
Solenoid valve is opened when 15Pa, is opened molecular pump and slide valve, is then proceeded to vacuumize；When chamber vacuum degree drops to 2 × 10-4
When, argon gas valve, shut-off valve and substrate spin valve are successively opened, is passed through argon gas that purity is 99.999% as sputter gas,
Argon gas valve flow is 12.5sccm, and substrate spins revolving speed as 1r/min；
Step 4: opening d.c. sputtering source, adjusting sputtering current is 0.1A, and adjusting slide valve is in sputtering pressure
0.15Pa is simultaneously sputtered, and sputtering time is 60 minutes；
Step 5: sputtering after successively close shielding power supply, shut-off valve, argon gas valve, substrate spin valve, slide valve,
Molecular pump, solenoid valve and mechanical pump are passed through nitrogen and open chamber door, take out sample to get dendroid amorphous MoS is arrived2Nanostructure,
To safeguard magnetron sputtering apparatus, cavity domestic demand extracts vacuum again.
Test example 2
The preparation method of this test example the following steps are included:
Step 1: substrate raw material is successively placed on acetone, dehydrated alcohol using quartz plate and electro-conductive glass as substrate raw material
Respectively it is cleaned by ultrasonic 20 minutes in solution, is then cleaned by ultrasonic 5 minutes in deionized water again, with being dried with nitrogen its surface moisture,
It is spare as sample substrate；
Step 2: being 99.99%, diameter 6cm by purity, with a thickness of the MoS of 5mm2Target is mounted on magnetic control sputtering device
No. 2 target position of device, then the quartz plate cleaned by step 1 and electro-conductive glass are fixed on disk with adhesive tape, electro-conductive glass is pre-
The surface area of 5mm × 5mm is stayed, while disk being fixed in revolvable base station, adjustment target-substrate distance is 10cm, disk plane
Angle with horizontal plane is 15 °；
Step 3: closing magnetron sputtering chamber door, mechanical pump is opened, to cavity vacuumize process, when cavity air pressure drops to
When 15Pa, solenoid valve is opened, molecular pump and slide valve is opened, then proceedes to vacuumize；When chamber vacuum degree drops to 2 × 10-4
When, argon gas valve, shut-off valve and substrate spin valve are successively opened, is passed through argon gas that purity is 99.999% as sputter gas,
Argon gas valve flow is 12.5sccm, and substrate spins revolving speed as 1r/min；
Step 4: opening d.c. sputtering source, adjusting sputtering current is 0.1A, and adjusting slide valve is in sputtering pressure
0.15Pa is simultaneously sputtered, and sputtering time is 40 minutes；
Step 5: sputtering after successively close shielding power supply, shut-off valve, argon gas valve, substrate spin valve, slide valve,
Molecular pump, solenoid valve and mechanical pump are passed through nitrogen and open chamber door, take out sample to get dendroid amorphous MoS is arrived2Nanostructure.
Step 6: for maintenance magnetron sputtering apparatus, cavity domestic demand extracts vacuum again.
Test example 3
The preparation method of this test example the following steps are included:
Step 1: substrate raw material is successively placed on acetone, dehydrated alcohol using quartz plate and electro-conductive glass as substrate raw material
Respectively it is cleaned by ultrasonic 20 minutes in solution, is then cleaned by ultrasonic 5 minutes in deionized water again, with being dried with nitrogen its surface moisture,
It is spare as sample substrate；
Step 2: being 99.99%, diameter 6cm by purity, with a thickness of the MoS of 5mm2Target is mounted on magnetic control sputtering device
No. 2 target position of device, then by after step 1 is cleaned quartz plate and electro-conductive glass be fixed on disk with adhesive tape, electro-conductive glass
The surface area of reserved 5mm × 5mm, while disk being fixed in revolvable base station, adjustment target-substrate distance is 10cm, and disk is flat
The angle of face and horizontal plane is 5 °；
Step 3: closing magnetron sputtering chamber door, mechanical pump is opened, to cavity vacuumize process, when cavity air pressure drops to
When 15Pa, solenoid valve is opened, molecular pump and slide valve is opened, then proceedes to vacuumize；When chamber vacuum degree drops to 2 × 10-4
When, argon gas valve, shut-off valve and substrate spin valve are successively opened, is passed through argon gas that purity is 99.999% as sputter gas,
Argon gas valve flow is 15sccm, and substrate spins revolving speed as 1r/min；
Step 4: opening d.c. sputtering source, adjusting sputtering current is 0.1A, and adjusting slide valve is in sputtering pressure
0.2Pa is simultaneously sputtered, and sputtering time is 60 minutes；
Step 5: sputtering after successively close shielding power supply, shut-off valve, argon gas valve, substrate spin valve, slide valve,
Molecular pump, solenoid valve and mechanical pump are passed through nitrogen and open chamber door, take out sample to get dendroid amorphous MoS is arrived2Nanostructure.
To safeguard magnetron sputtering apparatus, cavity domestic demand extracts vacuum again.
Test example 4
The preparation method of this test example the following steps are included:
Step 1: substrate raw material is successively placed on acetone, dehydrated alcohol using quartz plate and electro-conductive glass as substrate raw material
Respectively it is cleaned by ultrasonic 20 minutes in solution, is then cleaned by ultrasonic 5 minutes in deionized water again, with being dried with nitrogen its surface moisture,
It is spare as sample substrate；
Step 2: being 99.99%, diameter 6cm by purity, with a thickness of the MoS of 5mm2Target is mounted on magnetic control sputtering device
No. 2 target position of device, then the quartz plate cleaned by step 1 and electro-conductive glass are fixed on disk with adhesive tape, electro-conductive glass is pre-
The surface area of 5mm × 5mm is stayed, while disk being fixed on revolvable sample stage, adjustment target-substrate distance is 9cm, disk plane
Angle with horizontal plane is 5 °；
Step 3: closing magnetron sputtering chamber door, mechanical pump is opened, to cavity vacuumize process, when cavity air pressure drops to
When 15Pa, solenoid valve is opened, molecular pump and slide valve is opened, then proceedes to vacuumize；When chamber vacuum degree drops to 2 × 10-4
When, argon gas valve, shut-off valve and substrate spin valve are successively opened, is passed through the argon gas of high-purity as sputter gas, argon gas valve stream
Amount is 20sccm, and substrate spins revolving speed as 1r/min；
Step 4: opening d.c. sputtering source, adjusting sputtering current is 0.1A, and adjusting slide valve is in sputtering pressure
0.2Pa is simultaneously sputtered, and sputtering time is 50 minutes；
Step 5: sputtering after successively close shielding power supply, shut-off valve, argon gas valve, substrate spin valve, slide valve,
Molecular pump, solenoid valve and mechanical pump are passed through nitrogen and open chamber door, take out sample to get dendroid amorphous MoS is arrived2Nanostructure,
To safeguard magnetron sputtering apparatus, cavity domestic demand extracts vacuum again.
Test example 5
The preparation method of this test example the following steps are included:
Step 1: substrate raw material is successively placed on third using the quartz plate of regular shape and electro-conductive glass as substrate raw material
Respectively it is cleaned by ultrasonic 20 minutes in ketone, ethanol solution, then ultrasound 5 minutes in deionized water again, with being dried with nitrogen its table
Face moisture, it is spare as sample substrate；
Step 2: being 99.99%, diameter 6cm by purity, with a thickness of the MoS of 5mm2Target is mounted on magnetic control sputtering device
No. 2 target position of device, then the quartz plate cleaned up in step 1 and electro-conductive glass are fixed on disk with high temperature gummed tape, it is conductive
Glass reserves the surface area of 5mm × 5mm, while disk being fixed on rotatable sample stage, and adjustment target-substrate distance is 12cm, circle
The angle of disk plane and horizontal plane is 3 °；
Step 3: closing magnetron sputtering chamber door, mechanical pump is opened, to cavity vacuumize process, when cavity air pressure drops to
When 15Pa, solenoid valve is opened, molecular pump and slide valve is opened, then proceedes to vacuumize；When chamber vacuum degree drops to 2 × 10-4
When, argon gas valve, shut-off valve and substrate spin valve are successively opened, is passed through argon gas that purity is 99.999% as sputter gas,
Argon gas valve flow is 12.5sccm, and substrate spins revolving speed as 1r/min；
Step 4: opening d.c. sputtering source, adjusting sputtering current is 0.1A, and adjusting slide valve is in sputtering pressure
0.15Pa is simultaneously sputtered, and sputtering time is 90 minutes；
Step 5: sputtering after successively close shielding power supply, shut-off valve, argon gas valve, substrate spin valve, slide valve,
Molecular pump, solenoid valve and mechanical pump are passed through nitrogen and open chamber door, take out sample to get dendroid amorphous MoS is arrived2Nanostructure,
To safeguard magnetron sputtering apparatus, cavity domestic demand extracts vacuum again.
The test and characterization of catalysis material:
The model of the magnetron sputtering apparatus used in test example are as follows: SKY-450 type magnetic control sputtering device.Acquire 1 He of test example
Dendroid amorphous MoS made from test example 22Nanostructure, using scanning electron microscope to dendroid amorphous MoS made from test example 12
The surface topography and section nanostructure of nanostructure are characterized, as a result as depicted in figs. 1 and 2 respectively；Then UV- is used
6300 type ultraviolet-visible photometers are to dendroid amorphous MoS made from test example 12Nanostructure carries out absorption spectrum experiment,
Its optical property is characterized, as a result as shown in Figure 3 and Figure 4；The sulfuric acid electrolyte for configuring 1mol/L, using electrochemical operation
It stands to dendroid amorphous MoS made from test example 1 and 22Nanostructure carries out I-V test, and test results are shown in figure 5, to it
Electrical properties are characterized.Fig. 1 is to sputter when angle is 5 ° that dendroid amorphous MoS is made2The exterior view of nanostructure, Fig. 2 are
It sputters when angle is 5 ° and dendroid amorphous MoS is made2The sectional view of nanostructure, Fig. 3 are dendroid amorphous MoS2Nanostructure exists
Abosrption spectrogram in 200nm-1000nm wave-length coverage, Fig. 4 are dendroid amorphous MoS2Time of the nanostructure under 0V voltage
Current density plot figure, Fig. 5 are the dendroid amorphous MoS for sputtering angle and being 5 ° and 15 °2The I-V curve figure of nanostructure, Fig. 6
It is dendroid amorphous MoS of the present invention2The illustraton of model of nanostructure, it can be seen that there is dendroid amorphous MoS2Nanostructure can inhale
Visible light is received, the response of light is sensitive and stablizes, and has good photoelectric properties.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection scope of appended claims of the present invention
It is interior.
Claims (9)
1. one kind prepares dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, which is characterized in that with MoS2As
Target, substrate are arranged in closed environment using quartz plate as substrate for target, and adjustment the distance between substrate and target are
9cm~12cm, and the angle of substrate and horizontal plane is adjusted to 0 °~15 °, then by closed environment vacuumize process, closed
Ambient pressure is down to 2 × 10-4When, argon gas is passed through into closed environment as sputter gas；Then the air pressure of closed environment is controlled
For 0.15Pa~0.2Pa, magnetron sputtering is carried out by d.c. sputtering source, sputtering time is 40min~90min, obtains dendroid
Amorphous MoS2Nanostructure.
2. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the MoS2It is not less than 99.99% MoS using purity2。
3. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the quartz plate is first successively cleaned by ultrasonic in acetone, dehydrated alcohol, deionized water, is then dried with nitrogen, is remake
For substrate.
4. according to claim 3 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
Be, the quartz plate be successively cleaned by ultrasonic in acetone soln 20min, be cleaned by ultrasonic in ethanol solution 20min, go from
It is cleaned by ultrasonic 5min in solution in sub- water.
5. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the substrate spins in sputtering process.
6. according to claim 5 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the spin revolving speed of the substrate is 1r/min.
7. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the sputtering current in the d.c. sputtering source is 0.1A.
8. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, the flow of the argon gas is 12.5sccm~20sccm.
9. according to claim 1 prepare dendroid amorphous MoS based on magnetron sputtering method2The method of nanostructure, feature
It is, is prepared by magnetron sputtering apparatus.
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