CN104762608B - A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth - Google Patents
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of the controllable horizontal CdS nano-wire arrays of direction of growth, belong to One, Dimensional Semiconductor Nano Materials preparing technical field.The present invention realizes the Controllable growth in cadmium sulfide nano wires direction using a kind of simple method first, and obtained nanowire length can reach tens microns long, a diameter of 100 ran.The technology of the present invention is simple, easy to control, is easy to large-scale production and application.The designed technique and prepared finished product of the present invention will have important application value at the integrated aspect of basic physical study and nanoscale simultaneously.
Description
Technical field
The present invention relates to a kind of preparation method of the controllable horizontal CdS nano-wire arrays of direction of growth, belong to one-dimensional half
Conductor technical field of nanometer material preparation.
Technical background
Cadmium sulfide (CdS) is a kind of typical II-VII race's semiconducting compound, and its energy gap is 2.42eV at room temperature.
It has excellent luminescent properties and light transfer characteristic, in fields such as light emitting diode, solar cell, nanowire lasers
There is important application value.So far, people have been developed that the side of diversified synthesizing one-dimensional semiconductor nanowires
Method, such as traditional chemical vapour deposition technique, hydro-thermal method, physical extension method etc..Especially traditional chemical vapour deposition technique,
Because the direction of growth of the nano wire under the collective effect of the factors such as substrate lattice, air-flow, thermal agitation is unfixed, cause it
The orientation for the nano wire prepared is often rambling；This, which is that next step nanowire system is integrated, brings huge be stranded
It is difficult.
It yet there are no in the prior art and the relevant report that substrate prepares CdS nano-wire arrays done with sapphire.
The content of the invention：
In view of the shortcomings of the prior art, the present invention provides a kind of controllable horizontal CdS nano wires of the pure component direction of growth
The preparation method of array, high-quality horizontal CdS nano-wire arrays can not be prepared by one-step method in the prior art by solving
Problem.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, comprises the steps：
Using the horizontal pipe furnace with air inlet and gas outlet as reacting furnace, using surface with catalyst gold sapphire as
Substrate；Substrate is placed in the one end of reacting furnace close to gas outlet；CdS powder is placed in reacting furnace；Vacuumize, be passed through carrier gas,
It is 750-850 DEG C, preferably 770-830 DEG C, more preferably 790-810 DEG C, substrate to be warming up to the heating-up temperature of CdS powder
Heating-up temperature for 200-600 DEG C, be preferably 250-500 DEG C, more preferably 300-400 DEG C；Carrier gas carries CdS steams and existed
Deposited on substrate, obtain CdS nano wires, then furnace cooling, ultrasonic vibration obtains horizontal CdS nano-wire arrays on substrate；
The catalyst gold is in strip or spot distribution on sapphire；The flow of the carrier gas is 10-100sccm, is preferably 30-
80sccm, more preferably 40-60sccm；During deposition, air pressure in stove is controlled to be 100-700mbar, be preferably 350-
600mbar, more preferably 400-550mbar.
In the present invention, using sapphire of the surface with catalyst gold as substrate, carrying out annealing to substrate can protect
Demonstrate,prove more preferable effect；The condition of annealing is：500-800 DEG C of temperature, time 10-30min.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, the CdS powder it is pure
Degree >=99.99%；It is preferred that purity >=99.999%.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, controls the sedimentation time to be
1-3 hours.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, the ultrasonic vibration is,
The substrate that there are CdS nano wires will be deposited to be placed in isopropanol or deionized water, control ultrasonic power for 40-120W, the time is
1-5 minutes.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, obtains water on substrate
After flat CdS nano-wire arrays, cleaned with deionized water, dry the CdS nano-wire arrays grown in the horizontal direction.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, the surface carries and urged
The sapphire of agent gold is prepared by following proposal：
Using sapphire as substrate, first by sapphire carry out the high temperature anneal after, sapphire coat one layer of positivity or
Prepare the strip or dot pattern being sized after negative photoresist on this substrate by photoetching；Then in the base of preparation
The golden film that upper plating a layer thickness is 5-10nm on bottom；Plate after golden film, then substrate is immersed in 5- in 40-60 DEG C of acetone
10min, is rinsed well with deionized water, dried, you can obtain sapphire of the surface with catalyst gold；
Or
Using sapphire as substrate, first sapphire is carried out after the high temperature anneal, it is (poly- to coat one layer of PMMA in sapphire
Methyl methacrylate) after, the strip or dot pattern being sized are prepared in substrate using electron beam exposure；Then
Plating a layer thickness is 5-10nm golden film in above-mentioned substrate；Plate after golden film, then substrate is immersed in 40-60 DEG C of acetone
Middle 5-10min, is rinsed well with deionized water, dried, you can obtain sapphire of the surface with catalyst gold；The high temperature is moved back
The temperature of fire processing is 1200-1600 DEG C, and the time is 3-10 hours.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, the sapphire is carried out
The high temperature anneal is：In air atmosphere, annealed 3-10 hours in 1200-1600 DEG C.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, the carrier gas is argon gas
Or the mixed gas of argon gas and hydrogen.
A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth of the present invention, prepared cadmium sulfide
Nano-wire array is the horizontal line array that chemical formula is CdS.Its length is 10-50 microns, preferably 20-30 microns；Diameter
For 100-500nm, preferably 150-300nm.
Principle and advantage
The present invention cleverly make use of some faces of Sapphire Substrate to have thermal instability, can spontaneously form at high temperature
The characteristic of raceway groove.Pass through rational state modulator so that when chemical vapour deposition technique prepares nano wire, CdS nano wires to the greatest extent may be used
Can along parallel to substrate growth.Due to the particularity of substrate used, especially when there is the presence of raceway groove on substrate, nanometer
Line can direction growth of the prioritizing selection along raceway groove.Simultaneously along other directions grow CdS nano wires, due to and substrate combination
Power is weak (for along the nano wire parallel to substrate growth), it is easy to is handled by ultrasonic vibration, realizes itself and band
Parallel to the substrate separation of substrate growth CdS nano wires；So as to obtain horizontal CdS nano-wire arrays.
The technology of the present invention is simple, easy to control, mainly uses chemical vapor deposition method one-step synthesis level side
To CdS nano-wire arrays.The sample obtained is arranged into an array, and nanowire length is up to 50um.It is 488nm laser in wavelength
Excite down, it is observed that the luminescence generated by light crest for having halfwidth to be less than 20nm near 510nm, illustrates that obtained CdS receives
Nanowire arrays crystalline quality is good.The one dimension semiconductor nano-wire array of this high-crystallinity is prepared and system in micro-nano device
Major application will be had on integrated.
Brief description of the drawings：
Fig. 1 is the SEM photograph of the CdS nano wires prepared by comparative example 1；
Fig. 2 a are photo of the horizontal CdS nano-wire arrays under karr Zeiss light microscope prepared by embodiment 1；
Fig. 2 b are the SEM photograph of the horizontal CdS nano-wire arrays prepared by embodiment 1；
Fig. 2 c are the photoluminescence spectra figure of the horizontal CdS nano-wire arrays prepared by embodiment 1.
Photo after CdS sample dispersions of the Fig. 3 prepared by comparative example 2 under karr Zeiss light microscope.
Fig. 4 is device therefor of the present invention and its operating diagram.
The direction of growth that CdS nano wires prepared by conventional method are can be seen that from the SEM pictures in Fig. 1 is disorderly and unsystematic
's.
As can be seen that the CdS nano wires prepared by the present invention are grown along specific direction from Fig. 2 a and Fig. 2 b,
Nanowire length is up to 30um length.
From Fig. 2 c photoluminescence spectra as can be seen that the present invention prepared by CdS nano-wire arrays crystalline quality very
Height, with good optical property.
From figure 3, it can be seen that the CdS samples prepared are generally nanobelt, line is less.
From fig. 4, it can be seen that the quartz boat equipped with CdS medicines is located at the heated center position of horizontal pipe furnace, substrate slice
Low-temperature space one end positioned at the close gas outlet of tube furnace.
Embodiment：
The present invention is described further in conjunction with accompanying drawing：
Comparative example 1：It is substrate to take Si pieces, cuts into 10 × 10mm sizes, the supersound washing 20min in acetone soln, then
With deionized water rinsing, take out and dried in 50 DEG C of baking ovens.Then the method for deposited by electron beam evaporation plated film is deposited on a si substrate
10nm golden film.Take a certain amount of CdS medicines to be fitted into quartz boat, be placed on the center of tube furnace, Si substrates are placed on pipe
The low-temperature space of formula stove.Carrier gas is passed through, the central temperature for being warming up to tube furnace is 810 DEG C, now the temperature of Si substrates position
For 400 DEG C, isothermal reaction is for a period of time.After reaction terminates, heating furnace is naturally cooled into room temperature.Can under SEM
To find that the cadmium sulfide nano wires direction of growth prepared is rambling.
Comparative example 2：
Sapphire Substrate is taken, 10 × 10mm sizes are cut into, the supersound washing 20min in acetone soln, then use deionization
Water is rinsed, and is taken out and is dried in 50 DEG C of baking ovens.Sapphire Substrate is placed in high-temperature annealing furnace and is made annealing treatment (the temperature of annealing
Spend for 1200 DEG C, the time is 10h), then pass through light after one layer of negative photoresist (DNR-L300) of coating on substrate after annealing
It is engraved in the strip pattern that 5 × 50um is prepared in the Sapphire Substrate；Then plating a layer thickness is 10nm's over the substrate
Golden film；Plate after golden film, then substrate be immersed in 10min in 50 DEG C of acetone, rinsed well, dried with deionized water, you can
Obtain sapphire of the surface with catalyst gold.
Take a certain amount of CdS medicines to be fitted into quartz boat, be placed on the center of tube furnace, Sapphire Substrate is placed on pipe
The low-temperature space of formula stove.Vacuumize, the argon gas being passed through with 50sccm flow, it is 50mbar to control pressure, is warming up to tube furnace
Central temperature is 800 DEG C, and now the temperature of Sapphire Substrate position is 380 DEG C, after isothermal reaction 2h；Heating furnace is natural
It is cooled to room temperature.Obtained sample is taken out and disperses to observe on the cover slip, it is found that obtained sample is generally nanobelt, nano wire
It is less.
Embodiment 1：
Sapphire Substrate is taken, 10 × 10mm sizes are cut into, the supersound washing 20min in acetone soln, then use deionization
Water is rinsed, and is taken out and is dried in 50 DEG C of baking ovens.Sapphire Substrate is placed in high-temperature annealing furnace and is made annealing treatment (the temperature of annealing
Spend for 1200 DEG C, the time is 10h), then pass through light after one layer of negative photoresist (DNR-L300) of coating on substrate after annealing
It is engraved in the strip pattern that 5 × 50um is prepared in the Sapphire Substrate；Then plating a layer thickness is 10nm's over the substrate
Golden film；Plate after golden film, then substrate be immersed in 10min in 50 DEG C of acetone, rinsed well, dried with deionized water, you can
Obtain sapphire of the surface with catalyst gold.
Take a certain amount of CdS medicines to be fitted into quartz boat, be placed on the center of tube furnace, Sapphire Substrate is placed on pipe
The low-temperature space of formula stove.Vacuumize, the argon gas being passed through with 50sccm flow, it is 500mbar to control pressure, is warming up to tube furnace
Central temperature is 800 DEG C, and now the temperature of Sapphire Substrate position is 380 DEG C, after isothermal reaction 2h；Heating furnace is natural
It is cooled to room temperature.It is 40W that obtained sample, which is taken out, and is placed on ultrasound 1min ultrasonic powers in aqueous isopropanol, then uses deionized water
Cleaning, drying, you can the CdS nano-wire arrays grown in the horizontal direction.Photo under karr Zeiss light microscope is such as
Shown in Fig. 2 a；Fig. 2 b are the photos under corresponding SEM；Fig. 2 c are the luminescence generated by lights under 488nm laser excitations
Photo, the centre wavelength of spectrum is 510nm, and halfwidth is about 20nm, it can be seen that the crystallization of prepared CdS nano wires
Quality is good.
Embodiment 2：
Sapphire Substrate is taken, 10 × 5mm sizes are cut into, the supersound washing 20min in acetone soln, then use deionized water
Rinse, take out and dried in 50 DEG C of baking ovens.Sapphire Substrate is placed in high-temperature annealing furnace and is made annealing treatment (the temperature of annealing
For 1600 DEG C, the time is 3h), then existed on substrate after annealing after one layer of negative photoresist (DNR-L300) of coating by photoetching
5 × 50um strip pattern is prepared in the Sapphire Substrate；Then plating a layer thickness is 5nm golden film over the substrate；
Plate after golden film, then substrate is immersed in 10min in 50 DEG C of acetone, rinsed well, dried with deionized water, you can obtain table
Sapphire of the face with catalyst gold.
Take a certain amount of CdS medicines to be fitted into quartz boat, be placed on the center of tube furnace, Sapphire Substrate is placed on pipe
The low-temperature space of formula stove.Vacuumize, the argon gas being passed through with 40sccm flow, it is 550mbar to control pressure, is warming up to tube furnace
Central temperature is 810 DEG C, and now the temperature of Sapphire Substrate position is 400 DEG C, after isothermal reaction 1h；Heating furnace is natural
It is cooled to room temperature.Obtained sample is taken out to put ultrasound 1min ultrasonic powers in deionized water be 40W, then it is clear with deionized water
Wash, dry, obtain the nano-wire array of horizontal growth.Reaction time is short, and obtained nanowire length is relatively short.
Embodiment 3：
Sapphire Substrate is taken, 10 × 5mm sizes are cut into, the supersound washing 20min in acetone soln, then use deionized water
Rinse, take out and dried in 50 DEG C of baking ovens.Sapphire Substrate is placed in high-temperature annealing furnace and is made annealing treatment (the temperature of annealing
For 1400 DEG C, the time is 8h), then existed on substrate after annealing after one layer of negative photoresist (DNR-L300) of coating by photoetching
5 × 50um strip pattern is prepared in the Sapphire Substrate；Then plating a layer thickness is 8nm golden film over the substrate；
Plate after golden film, then substrate is immersed in 10min in 50 DEG C of acetone, rinsed well, dried with deionized water, you can obtain table
Sapphire of the face with catalyst gold.
Take a certain amount of CdS medicines to be fitted into quartz boat, be placed on the center of tube furnace, Sapphire Substrate is placed on pipe
The low-temperature space of formula stove.Vacuumize, the argon gas being passed through with 60sccm flow, it is 400mbar to control pressure, is warming up to tube furnace
Central temperature is 790 DEG C, and now the temperature of Sapphire Substrate position is 350 DEG C, after isothermal reaction 1h；Heating furnace is natural
It is cooled to room temperature.Obtained sample is taken out to put ultrasound 1min ultrasonic powers in deionized water be 40W, then it is clear with deionized water
Wash, dry, obtain the nano-wire array of horizontal growth.
From embodiment 1 and comparative example 2 it can be seen that in the selection of substrate, CdS powder evaporating temperature, depositing temperature, carrier gas
Under flow, the synergy of furnace pressure, the horizontal CdS nano-wire arrays of high-quality can be just obtained.In comparative example 2, due to heavy
During product, furnace pressure causes gained sample mostly nanobelt not in limited range of the present invention, and nano wire is less.
Claims (6)
1. a kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth, it is characterised in that comprise the steps：
Using the horizontal pipe furnace with air inlet and gas outlet as reacting furnace, using sapphire of the surface with catalyst gold as lining
Bottom；Substrate is placed in the one end of reacting furnace close to gas outlet；CdS powder is placed in reacting furnace；Vacuumize, be passed through carrier gas, rise
Temperature to the heating-up temperature of CdS powder is 750-850 DEG C, and the heating-up temperature of substrate is 200-400 DEG C；Carrier gas carries CdS steams and existed
Deposited on substrate, obtain CdS nano wires, then furnace cooling, ultrasonic vibration obtains horizontal CdS nano-wire arrays on substrate；
The catalyst gold is in strip or spot distribution on sapphire；The flow of the carrier gas is 10-100sccm；During deposition, control
Air pressure is 100-700mbar in stove processed；
Sapphire of the surface with catalyst gold is prepared by following proposal：
Using sapphire as substrate, first sapphire is carried out after the high temperature anneal, one layer of positivity of coating or negative photoresist lead to
Cross photoetching and the golden film that plating a layer thickness after the strip being sized or dot pattern is 5-10nm is prepared in substrate；Plating
After upper golden film, then substrate is immersed in 5-10min in 40-60 DEG C of acetone, rinsed well with deionized water, dry and can obtain
Sapphire of the surface with catalyst gold；
Or
Using sapphire as substrate, first sapphire is carried out after the high temperature anneal, one layer of PMMA is coated, using electron beam exposure
Method prepares the golden film that plating a layer thickness after the strip being sized or dot pattern is 5-10nm in substrate；Plate
After golden film, then substrate is immersed in 5-10min in 40-60 DEG C of acetone, rinsed well with deionized water, dry and can obtain table
Sapphire of the face with catalyst gold；
Sapphire carries out the high temperature anneal, in air atmosphere, is annealed 3-10 hours in 1200-1600 DEG C.
2. a kind of preparation method of the controllable horizontal CdS nano-wire arrays of direction of growth according to claim 1, it is special
Levy and be：Purity >=99.99% of the CdS powder.
3. a kind of preparation method of the controllable horizontal CdS nano-wire arrays of direction of growth according to claim 2, it is special
Levy and be：Using the horizontal pipe furnace with air inlet and gas outlet as reacting furnace, using surface with catalyst gold sapphire as
Substrate；Substrate is placed in the one end of reacting furnace close to gas outlet；CdS powder is placed in reacting furnace；Vacuumize, be passed through carrier gas,
The heating-up temperature for being warming up to CdS powder is 770-830 DEG C, and the heating-up temperature of substrate is 250-400 DEG C；Carrier gas carries CdS steams
Deposited on substrate, obtain CdS nano wires, then furnace cooling, ultrasonic vibration obtains horizontal CdS nanometers of linear array on substrate
Row；The catalyst gold is in strip or spot distribution on sapphire；The flow of the carrier gas is 30-80sccm；During deposition,
It is 350-600mbar to control air pressure in stove.
4. a kind of preparation method of the controllable horizontal CdS nano-wire arrays of direction of growth according to claim 3, it is special
Levy and be：Using the horizontal pipe furnace with air inlet and gas outlet as reacting furnace, using surface with catalyst gold sapphire as
Substrate；Substrate is placed in the one end of reacting furnace close to gas outlet；CdS powder is placed in reacting furnace；Vacuumize, be passed through carrier gas,
The heating-up temperature for being warming up to CdS powder is 790-810 DEG C, and the heating-up temperature of substrate is 300-400 DEG C；Carrier gas carries CdS steams
Deposited on substrate, obtain CdS nano wires, then furnace cooling, ultrasonic vibration obtains horizontal CdS nanometers of linear array on substrate
Row；The catalyst gold is in strip or spot distribution on sapphire；The flow of the carrier gas is 40-60sccm；；Deposition
When, it is 400-550mbar to control air pressure in stove.
5. a kind of system of the controllable horizontal CdS nano-wire arrays of direction of growth according to claim 1-4 any one
Preparation Method, it is characterised in that：It is 1-3 hours to control sedimentation time.
6. a kind of system of the controllable horizontal CdS nano-wire arrays of direction of growth according to claim 1-4 any one
Preparation Method, it is characterised in that：The ultrasonic vibration is that the substrate that deposition has CdS nano wires is placed in into isopropanol or deionization
In water, it is 40-120W to control ultrasonic power, and the time is 1-5 minutes.
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| CN105926034B (en) * | 2016-06-21 | 2018-03-27 | 中国科学院理化技术研究所 | A kind of preparation method of CdS or CdSe monocrystal nano line arrays |
| CN109250924B (en) * | 2018-12-07 | 2021-05-14 | 香港中文大学（深圳） | Method for rapidly preparing organic micromolecule nano-rod |
| CN109881247B (en) * | 2019-03-14 | 2020-05-22 | 北京大学 | Preparation method of bent SnTe single crystal nanowire |
| CN113667937B (en) * | 2021-07-30 | 2023-06-06 | 华南师范大学 | Alq 3 Preparation method and application of nanowire horizontal array |
| CN113894018B (en) * | 2021-09-26 | 2023-02-24 | 华南师范大学 | Method for forming organic nanowire on surface of flexible substrate, organic nanowire and application thereof |
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