CN110040762A - A method of growing zinc oxide nanorod arrays are regulated and controled based on two-dimensional colloidal monofilm - Google Patents
A method of growing zinc oxide nanorod arrays are regulated and controled based on two-dimensional colloidal monofilm Download PDFInfo
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Abstract
The invention discloses a kind of method based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays, this method prepares height and the adjustable nanometic zinc oxide rod array of hydrophilic and hydrophobic using two-dimensional colloidal monofilm as template, by hydro-thermal method.The method of the present invention is simple and quick, the different hydrothermal growth time available nanometic zinc oxide rod arrays with different height, the nanometic zinc oxide rod array of different height has different hydrophilic and hydrophobics, realize the regulation in lower temperature, shorter reaction time to nanometic zinc oxide rod array, and constructed nanometic zinc oxide rod array has fabulous stability, all has potential application in surface-enhanced Raman, bio-medical, nanophotonics, electro-catalysis and new energy application aspect.
Description
Technical field
Technical field is constructed the invention belongs to semiconductor nanorods array structure, and in particular to one kind is with two-dimensional colloidal list
Tunic is the method that template regulates and controls nanometic zinc oxide rod array structure growth.
Background technique
Zinc oxide (ZnO) is a kind of important semiconductor material, has broad stopband (3.37eV) and high exciton binding energy
(60meV) has good piezoelectricity, electric conductivity, the transparency and photoelectron performance etc., thus in catalysis, solar battery, pressure
The fields such as electrical part, biomedical sensing and micro-/ nano electronics are with a wide range of applications.Nano ZnO has a variety of
The performances such as pattern, high chemical stability, adjustable photoelectric properties and good biocompatibility, it can be used as surface enhanced drawing
The superior substrate material of graceful scattering (SERS).Wherein, the ZnO nanorod with array structure is due to surface volume with higher
Than many advantages, such as, pattern is easy to regulate and control, the speed of growth is fast and at low cost, it has also become there is high activity, high stability and can weigh
The preferred SERS active-substrate material of multiple usability.
Under normal conditions, researchers prepare nanometic zinc oxide rod array structure by different synthetic technologys, including change
Learn the hydrothermal growth process etc. in vapor deposition (CVD), electro-deposition, pulsed laser deposition and liquid medium.CVD method preparation oxidation
Zinc nanometer rods be using zinc simple substance or zinc oxide as raw material in tube furnace in vapor reaction, through pervaporation or redox,
It decomposes and the chemical processes such as chemical combination prepares zinc oxide nano rod.CVD method is generally required to be carried out under 500 DEG C or more high temperature,
The factors such as type, partial pressure, flow velocity and the catalyst type of control reaction temperature and reaction gas are also needed to a certain extent, it is difficult to real
Existing large scale preparation.Electro-deposition techniques are using substrate to be grown as the working electrode in electrochemical cell, are pair with graphite plate
Electrode, electrolyte are the aqueous solution containing zinc salt (such as zinc nitrate) and potassium chloride, are carried out under the conditions of a constant current and temperature
Deposition, electro-deposition techniques can regulate and control the growth of zinc oxide nano rod by current time and electrolyte concentration.Electrochemical deposition
Deficiency existing for method is can not to obtain ZnO nano material on a dielectric base.Pulsed laser deposition utilizes pulse laser
Raw material are evaporated the method for being deposited as nano material by high-energy, and the ratio of width to height for being orientated good controlled diameter can be made
At least 50 nano-wire array, its advantage is that the shape and surface to target are easy to adulterate without particular/special requirement, deposition efficiency is high,
But higher sedimentary condition, the factors such as laser power density, reaction temperature and depositing temperature to construct zinc oxide nano rod
Array structure it is inefficient, and cost is very high.Hydrothermal growth process refer to it is a kind of in the pressure vessel of sealing, using water as molten
Agent generates high temperature and high pressure environment by the way that reaction system is added, and accelerates ionic reaction and promotes hydrolysis, makes in aqueous solution
The method of standby metal oxide, zinc oxide nano rod made from hydro-thermal method have that crystal grain is complete, granularity is small, particle agglomeration is relatively light and
The characteristics of being evenly distributed, it can be achieved that at a lower temperature, without special installation, facilitate large scale preparation.
In addition to above method, with porous aluminas, silicon nanowires, graphene and colloidal crystal etc. for template, template is utilized
Cellular structure and regular pattern etc. the accurate control synthesis of zinc oxide nano rod may be implemented.For example, Hou et al. (The
Journal of Physical Chemistry B, 2004,108 (32): 11976-11980.) utilize porous aluminas array
It is 130nm and 260nm, 7.6~14 μm of length that structure, which is prepared for diameter by the method evaporated under the conditions of 700~900 DEG C,
Nanometic zinc oxide rod array structure.Kang et al. (Sensors and Actuators B:Chemical, 2018,273:48-
55.) it reports and grows branch shaped zinc oxide nanometer stick array structure on Si nanowire array structure by hydro-thermal method, form cladodification
Draw ratio perpendicular to Si nano wire is about 20 nanometic zinc oxide rod array structures, but constructing for Si nano-wire array matrix need to adopt
It is performed etching with solution such as hydrofluoric acid, there is certain risk.He et al. (Journal of The Electrochemical
Society, 2017,164 (13) D895-D900.) report using Hexagonal packing polystyrene two-dimensional array structure be mould
Plate, the method growing zinc oxide nanorod structure of electro-deposition, by the concentration of electrolyte solution in control reaction process to obtain
The nanometic zinc oxide rod array structure of different length, zinc oxide nano rod diameter is about 150nm, length is about 1 μm, but electro-deposition
The experimental provision of technology high requirement can not make its large scale preparation.Zhang group (Dalton Trans., 2015,44,
3447-3453.) using the patterned sapphire substrate with hemispherical array, by conventional hydrothermal growth process in substrate surface
High-sequential nanometic zinc oxide rod array structure is constructed, nanometer rods are about 1 μm long, diameter is about 60nm, patterned sapphire half
The distance between ball can regulate and control the growth of nanometer stick array structure, but the needs of constructing of sapphire hemisphere substrate are spent compared with great achievement
This.Du et al. (Applied Physics, A 2019,125:138.) utilizes dimethyl silicone polymer (PDMS) flexible substrates system
For three-dimensional classification zinc oxide dewatering nano structure, adjusts hydrothermal reaction condition and obtain the flexibility with different surface morphology structure
Active substrate, nanorod structure all has preferable homogeneity and length, but the irregular structure on PMDS flexible matrix surface is not
It can be as the optimal Template of array structure growth.
Summary of the invention
The object of the present invention is to provide one kind using two-dimensional colloidal monofilm as template, is prepared by hydro-thermal method highly and close and distant
The method of aqueous adjustable nanometic zinc oxide rod array.
For above-mentioned purpose, the technical solution adopted in the present invention is made of following step:
1, two-dimensional colloidal monofilm is prepared
Using water and ethyl alcohol volume ratio for 1:1~10:1 mixed liquor as solvent, by the poly- (styrene-N- isopropyl of core-shell type
Acrylamide)@polyacrylic acid be configured to mass percent be 1%~10% suspension；It is in 30~60 ° by sheet glass and liquid level
It is inserted into 0.01~0.08mmol/L lauryl sodium sulfate aqueous solution, then gained hanging drop is added on sheet glass, is made
It is distributed on gas-liquid interface along sheet glass, forms closely packed two-dimensional colloidal monofilm；Finally, the two-dimentional glue that interface is formed
Body monofilm is transferred to hydrophilic base surface, dries under natural conditions.
2, nanometic zinc oxide rod array is constructed
The hydrophilic base that the surface that step 1 is obtained is placed with two-dimensional colloidal monofilm is hydrated in 5~20mmol/L bis-
It is taken out after impregnating 3~6h in the ethanol solution of zinc acetate, 70~90 DEG C of drying lie against in hydrothermal reaction kettle, there is the one side of film
Upward；Urotropine is added into 10~50mmol/L zinc nitrate hexahydrate aqueous solution, is added after stirring and dissolving poly-
Aziridine, and pH=9~12 are adjusted with ammonium hydroxide, it is subsequently poured into above-mentioned hydrothermal reaction kettle, 85~95 DEG C in confined conditions
10~180min of hydrothermal growth, obtains nanometic zinc oxide rod array.
In above-mentioned steps 1, preferably using water and ethyl alcohol volume ratio for 1:1~5:1 mixed liquor as solvent, core-shell type is gathered
(styrene-n-isopropyl acrylamide)@polyacrylic acid is configured to the suspension that mass percent is 3%~6%.
It is in further preferably 30~60 ° of insertion 0.03~0.05mmol/L 12 by sheet glass and liquid level in above-mentioned steps 1
In alkylsurfuric acid sodium water solution, then gained hanging drop is added on sheet glass, it is made to be distributed to gas-liquid interface along sheet glass
On, form closely packed two-dimensional colloidal monofilm.
In above-mentioned steps 1, the hydrophilic base is that the mixed liquor for being 7:3 through the concentrated sulfuric acid and concentrated nitric acid volume ratio is handled
Silicon wafer, quartz plate, ITO electro-conductive glass, any one in FTO electro-conductive glass.
In above-mentioned steps 2, surface is preferably placed with the hydrophilic base of two-dimensional colloidal monofilm in 10~15mmol/L
It is taken out after impregnating 5h in the ethanol solution of Zinc diacetate dihydrate, 90 DEG C of drying.
In above-mentioned steps 2, urotropine preferably is added into 20~30mmol/L zinc nitrate hexahydrate aqueous solution,
Polyethyleneimine is added after stirring and dissolving, and adjusts pH=10~11 with ammonium hydroxide, wherein the zinc nitrate hexahydrate and ring six
Methenamine, polyethyleneimine molar ratio be 1:1~1.2:0.1~0.2, the number-average molecular weight of the polyethyleneimine is
10000~30000.
In above-mentioned steps 2, preferably in confined conditions 90 DEG C of 30~120min of hydrothermal growth.
The two-dimensional colloidal monofilm that the present invention is constructed using polymer-network method prepares zinc oxide nano by hydro-thermal method as template
Rice stick array, realizes the regulation in lower temperature, shorter reaction time to nanometic zinc oxide rod array.When by regulation reaction
Between, height can be obtained in the nanometic zinc oxide rod array of 200~1000nm range, and with the increase of nanometer rods height, battle array
Column are gradually converted into hydrophobicity by hydrophily.The size of polymer-network method construction unit determines the intensive of zinc oxide nano rod
The construction unit of degree, different-grain diameter can obtain the nanometic zinc oxide rod array with different-shape structure.
The method of the present invention is simple and quick, and constructed nanometic zinc oxide rod array has fabulous stability, on surface
Enhancing Raman, bio-medical, nanophotonics, electro-catalysis and new energy application aspect all have potential application.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph for the two-dimensional colloidal monofilm that embodiment 1 obtains.
Fig. 2 is the electron scanning micrograph in the two-dimensional colloidal monofilm section that embodiment 1 obtains.
Fig. 3 is the XRD diagram that the nanometic zinc oxide rod array of 30min is grown in embodiment 1.
Fig. 4 is the electron scanning micrograph that the nanometic zinc oxide rod array of 30min is grown in embodiment 1.
Fig. 5 is the cross sectional scanning electron microscope and contact angle that the nanometic zinc oxide rod array of 30min is grown in embodiment 1
Photo.
Fig. 6 is the electron scanning micrograph that the nanometic zinc oxide rod array of 60min is grown in embodiment 2.
Fig. 7 is the cross sectional scanning electron microscope and contact angle that the nanometic zinc oxide rod array of 60min is grown in embodiment 2
Photo.
Fig. 8 is the electron scanning micrograph that the nanometic zinc oxide rod array of 120min is grown in embodiment 3.
Fig. 9 is cross sectional scanning electron microscope and the contact that the nanometic zinc oxide rod array of 120min is grown in embodiment 3
Angle photo.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Poly- (styrene-n-isopropyl acrylamide)@polyacrylic acid (P (St-co- of core-shell type used in embodiment
NIPAM)@PAA) according to document " Colloid and Polymer Science, 2015,293 (8): the side in 2405-2417. "
Method synthesis, specific synthetic method are as follows: be dissolved in 0.20g n-isopropyl acrylamide (NIPAM) and 1.80g styrene (St)
In 90mL deionized water, the heating water bath under nitrogen atmosphere protection and mechanical stirring (constant 400r/min revolving speed), to system temperature
Degree rises to 70 DEG C, is 5.92 × 10 by 10mL concentration-2Reaction system is added in mol/L persulfate aqueous solution, and polymerization reaction 8h is obtained
To P (St-co-NIPAM) microballoon dispersion liquid；By 1.0g acrylic acid (AA) monomer and 0.1g N, N '-methylene-bisacrylamide
(MBA) it is dissolved in 10mL distilled water, is then added in P (St-co-NIPAM) microballoon dispersion liquid, and 3mL concentration is added and is
9.86×10-2Mol/L persulfate aqueous solution, it is 70 DEG C lower in nitrogen atmosphere protection and mechanical stirring (constant 400r/min revolving speed)
4h is heated in water bath with thermostatic control, is cooled to room temperature, and product alternately washs, after centrifugation (revolving speed 9000r/min) through water and dehydrated alcohol,
Freeze-drying, obtains P (St-co-NIPAM)@PAA, and size is uniform, and partial size is 300nm or so.
Embodiment 1
1, two-dimensional colloidal monofilm is prepared
Using water and ethyl alcohol volume ratio for 1:1 mixed liquor as solvent, P (St-co-NIPAM)@PAA is configured to quality hundred
Divide the suspension than being 4%；It is in 45 ° of insertion 500mL 0.04mmol/L lauryl sodium sulfate aqueous solutions by sheet glass and liquid level
In, then gained hanging drop is added on sheet glass, is distributed to it on gas-liquid interface along sheet glass, forms closely packed two
Tie up colloid monolayers film.Finally, it is 7:3 that the two-dimensional colloidal monofilm that interface is formed, which is transferred to through the concentrated sulfuric acid and concentrated nitric acid volume ratio,
Mixed liquor processing the surface silicon wafer (1cm × 1cm), dry under natural conditions.It is scanned using Hitachi SU8220 type awkward silence at a meeting
Electron microscope observation sample topography structure, by Fig. 1~2 as it can be seen that P (St-co-NIPAM)@PAA is tightly packed in six side of single layer
It is arranged in silicon chip surface.
2, nanometic zinc oxide rod array is constructed
Surface is placed with to ethanol solution of the silicon wafer in 10mL 10mmol/L Zinc diacetate dihydrate of two-dimensional colloidal monofilm
It is taken out after middle immersion 5h, 90 DEG C of drying lie against in 50mL hydrothermal reaction kettle, have the one side of film upward；It is added into 40mL water
0.298g (25mmol) zinc nitrate hexahydrate, 0.14g (25mmol) urotropine add 0.135g after stirring and dissolving
The polyethyleneimine that (3mmol) number-average molecular weight is 10000, and pH=10.5 is adjusted with ammonium hydroxide, it is subsequently poured into hydrothermal reaction kettle
In, 90 DEG C of hydrothermal growth 30min, obtain nanometic zinc oxide rod array (P (St-co-NIPAM)@PAA/ in confined conditions
ZnONRs)。
Using the crystalline structure of full-automatic (Bruker D8Discover) the X-ray diffractometer measurement sample of Brooker,
Hitachi SU8220 type awkward silence at a meeting scanning electron microscope observes sample topography structure and Dataphysics company, Germany OCA 20
Type video optics contact angle measurement, is as a result shown in Fig. 3~5.As seen from Figure 3, the lattice that zinc oxide nano rod occurs in sample spreads out
It penetrates, it was demonstrated that zinc oxide nano rod is successfully prepared.By Fig. 4 and Fig. 5 as it can be seen that the growing height of zinc oxide nano rod is about
203.8nm, surface contact angle are 44.3 °.
Embodiment 2
In the step 2 of the present embodiment, 90 DEG C of hydrothermal growth 60min in confined conditions, other steps and 1 phase of embodiment
Together, nanometic zinc oxide rod array is obtained.By Fig. 6 and Fig. 7 as it can be seen that the growing height of zinc oxide nano rod is 543.7nm, contact angle
It is 85.6 °.
Embodiment 3
In the step 2 of the present embodiment, 90 DEG C of hydrothermal growth 120min in confined conditions, other steps and 1 phase of embodiment
Together, nanometic zinc oxide rod array is obtained.By Fig. 8 and Fig. 9 as it can be seen that the growing height of zinc oxide nano rod is 1013.2nm, contact
Angle is 123.7 °.
Embodiment 4
1, two-dimensional colloidal monofilm is prepared
Using water and ethyl alcohol volume ratio for 5:1 mixed liquor as solvent, P (St-co-NIPAM)@PAA is configured to quality hundred
Divide the suspension than being 6%；It is in 60 ° of insertion 500mL 0.05mmol/L lauryl sodium sulfate aqueous solutions by sheet glass and liquid level
In, then gained hanging drop is added on sheet glass, is distributed to it on gas-liquid interface along sheet glass, forms closely packed two
Tie up colloid monolayers film.Finally, by interface formed two-dimensional colloidal monofilm be transferred to handled through Piranha acid silicon wafer (1cm ×
1cm) surface is dried under natural conditions.
2, nanometic zinc oxide rod array is constructed
Surface is placed with to ethanol solution of the silicon wafer in 10mL 15mmol/L Zinc diacetate dihydrate of two-dimensional colloidal monofilm
It is taken out after middle immersion 5h, 90 DEG C of drying lie against in 50mL hydrothermal reaction kettle, have the one side of film upward；It is added into 40mL water
0.238g (20mmol) zinc nitrate hexahydrate, 0.112g (20mmol) urotropine add after stirring and dissolving
The polyethyleneimine that 0.108g (2.4mmol) number-average molecular weight is 10000, and pH=9 is adjusted with ammonium hydroxide, it is anti-to be subsequently poured into hydro-thermal
It answers in kettle, 90 DEG C of hydrothermal growth 60min, obtain nanometic zinc oxide rod array in confined conditions.
Embodiment 5
1, two-dimensional colloidal monofilm is prepared
Using water and ethyl alcohol volume ratio for 3:1 mixed liquor as solvent, P (St-co-NIPAM)@PAA is configured to quality hundred
Divide the suspension than being 3%；It is in 30 ° of insertion 500mL0.03mmol/L lauryl sodium sulfate aqueous solutions by sheet glass and liquid level
In, then gained hanging drop is added on sheet glass, is distributed to it on gas-liquid interface along sheet glass, forms closely packed two
Tie up colloid monolayers film.Finally, by interface formed two-dimensional colloidal monofilm be transferred to handled through Piranha acid silicon wafer (1cm ×
1cm) surface is dried under natural conditions.
2, nanometic zinc oxide rod array is constructed
Surface is placed with to ethanol solution of the silicon wafer in 10mL 10mmol/L Zinc diacetate dihydrate of two-dimensional colloidal monofilm
It is taken out after middle immersion 5h, 90 DEG C of drying lie against in 50mL hydrothermal reaction kettle, have the one side of film upward；It is added into 40mL water
0.358g (30mmol) zinc nitrate hexahydrate, 0.168g (30mmol) urotropine add after stirring and dissolving
The polyethyleneimine that 0.162g (3.6mmol) number-average molecular weight is 10000, and pH=11 is adjusted with ammonium hydroxide, it is subsequently poured into hydro-thermal
In reaction kettle, 90 DEG C of hydrothermal growth 120min, obtain nanometic zinc oxide rod array in confined conditions.
Claims (9)
1. it is a kind of based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays method, it is characterised in that this method by
Following step composition:
(1) two-dimensional colloidal monofilm is prepared
Using water and ethyl alcohol volume ratio for 1:1~10:1 mixed liquor as solvent, by the poly- (styrene-N- isopropyl propylene of core-shell type
Amide)@polyacrylic acid be configured to mass percent be 1%~10% suspension；By sheet glass and liquid level in 30~60 ° of insertions
In 0.01~0.08mmol/L lauryl sodium sulfate aqueous solution, then gained hanging drop is added on sheet glass, makes its edge
Sheet glass is distributed on gas-liquid interface, forms closely packed two-dimensional colloidal monofilm；Finally, the two-dimensional colloidal list that interface is formed
Tunic is transferred to hydrophilic base surface, dries under natural conditions；
(2) nanometic zinc oxide rod array is constructed
The hydrophilic base that the surface that step (1) obtains is placed with two-dimensional colloidal monofilm is hydrated vinegar in 5~20mmol/L bis-
It is taken out after impregnating 3~6h in the ethanol solution of sour zinc, 70~90 DEG C of drying lie against in hydrothermal reaction kettle, have the one of film to face
On；Urotropine is added into 10~50mmol/L zinc nitrate hexahydrate aqueous solution, poly- second is added after stirring and dissolving
Alkene imines, and pH=9~12 are adjusted with ammonium hydroxide, it is subsequently poured into above-mentioned hydrothermal reaction kettle, in confined conditions 85~95 DEG C of water
Thermally grown 10~180min, obtains nanometic zinc oxide rod array.
2. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
Be characterized in that: in step (1), using water and ethyl alcohol volume ratio for 1:1~5:1 mixed liquor as solvent, by poly- (the benzene second of core-shell type
Alkene-n-isopropyl acrylamide)@polyacrylic acid be configured to mass percent be 3%~6% suspension.
3. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
It is characterized in that: being in 30~60 ° of insertion 0.03~0.05mmol/L lauryl sodium sulfate by sheet glass and liquid level in step (1)
In aqueous solution, then gained hanging drop is added on sheet glass, is distributed to it on gas-liquid interface along sheet glass, forms Mi Dui
Long-pending two-dimensional colloidal monofilm.
4. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
Be characterized in that: in step (1), the hydrophilic base is that the mixed liquor for being 7:3 through the concentrated sulfuric acid and concentrated nitric acid volume ratio is handled
Silicon wafer, quartz plate, ITO electro-conductive glass, any one in FTO electro-conductive glass.
5. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
It is characterized in that: in step (2), the hydrophilic base that surface is placed with two-dimensional colloidal monofilm being hydrated in 10~15mmol/L bis-
It is taken out after impregnating 5h in the ethanol solution of zinc acetate, 90 DEG C of drying.
6. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
It is characterized in that: in step (2), urotropine is added into 20~30mmol/L zinc nitrate hexahydrate aqueous solution, stir
Polyethyleneimine is added after dissolution, and adjusts pH=10~11 with ammonium hydroxide.
7. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
Be characterized in that: in step (2), the zinc nitrate hexahydrate and urotropine, polyethyleneimine molar ratio be 1:1~
1.2:0.1~0.2.
8. the method according to claim 7 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
Be characterized in that: in step (2), the number-average molecular weight of the polyethyleneimine is 10000~30000.
9. the method according to claim 1 based on two-dimensional colloidal monofilm regulation growing zinc oxide nanorod arrays,
It is characterized in that: in step (2), 90 DEG C of 30~120min of hydrothermal growth in confined conditions.
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| CN110656328A (en) * | 2019-08-29 | 2020-01-07 | 湖北大学 | Preparation method of Janus foam copper with asymmetric wettability and efficient mist collection capacity |
| CN111945141A (en) * | 2020-08-13 | 2020-11-17 | 湖北大学 | Preparation method of multifunctional super-smooth surface based on hollow zinc oxide nano structure |
| TWI801776B (en) * | 2020-11-24 | 2023-05-11 | 國立聯合大學 | Producing method of pd-adsorbed zno nanostructures |
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