CN107628635B - A kind of method and nano zine oxide of hydrothermal synthesis four-blade propeller shape nano zine oxide - Google Patents
A kind of method and nano zine oxide of hydrothermal synthesis four-blade propeller shape nano zine oxide Download PDFInfo
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Abstract
The invention discloses the method and nano zine oxide of a kind of hydrothermal synthesis four-blade propeller shape nano zine oxide, step 1: at 20 DEG C, the Zn (NO of 1.0mmol is weighed3)2·6H240.0mL deionized water is added in beaker in the NaOH of O and 20.0mmol, is placed in the SDS of addition 1.0mmol after magnetic stirrer, continues 2-3 hour of stirring to solution and is uniformly mixed;Step 2: above-mentioned solution is moved in reaction kettle, is placed in 200 DEG C of thermostatic drying chamber and is kept the temperature for 24 hours;Step 3: after reaction, after reaction kettle is cooled to room temperature with tap water, reaction kettle is opened;Step 4: solution left standstill, precipitating, separation are washed 3 times with dehydrated alcohol, obtain white four-blade propeller shape zinc oxide nano powder.Li Shui of the present invention is solvent, using soluble zinc nitrate as zinc source, using SDS as pattern to directed agents, and one-step synthesis four-blade propeller shape nano zine oxide.
Description
Technical field
The invention belongs to semiconductor nano material preparation fields, and it is nano oxidized to be related to a kind of hydrothermal synthesis four-blade propeller shape
The method and nano zine oxide of zinc.
Background technique
Zinc oxide is the second B metal oxide, is a kind of N-type wide-band-gap semiconductor material, and forbidden bandwidth reaches
3.37eV has chemical and thermal stability, photoelectricity and piezoelectric property not available for general material, is a kind of multifunctional usage
Material, is quite suitable for the application in terms of high-and-new science and technology, and relatively common has light emitting diode, photodetector and photoelectricity
The optical modulator etc. of diode.Nano zinc oxide material is again due to its unique surface and interfacial effect, small-size effect, quantum
Dimensional effect and macro quanta tunnel effect, thus, electricity, magnetics, optics, mechanics and in terms of show it is very excellent
Different performance, while it is many also by more and more scholars to be widely applied to sewage treatment, sensor and solar battery etc.
Field.
Due to its unique optical property, in addition in the side such as light emitting diode, ultraviolet light detector and ultraviolet laser device
There are many applications in face;Also occupy irreplaceable role in terms of uvioresistant and photocatalytic degradation.Furthermore militarily
Absorbing radar wave and for shielding ultraviolet rays and absorb infrared light building inside and outside wall lotion in coating can aspect have
It is widely applied.Based on the distinctive chemical property of zinc oxide and semiconducting behavior, in terms of photosensitizer is catalyzed solar battery
Surface goes out good prospect.Additionally due to its under ultraviolet light irradiation, make its in water with can allow substance decomposition output in air
Free-moving electrons and holes, this hole can activate the oxygen in air, so that it becomes active oxygen, has extremely strong chemistry
Activity is directly applied to sterilization, disinfection, deodorization in terms of biologic pharmacological science, while being also applied to examine as semiconductor material
In terms of the biosensor for surveying glucolase, the specific target molecule of identification and detection nerve cell activity voltage etc..Though
Right nano zine oxide has various excellent performances, but also has with the pattern result of its own and closely contact.In recent years, state
It is inside and outside to have had developed a variety of zinc oxide appearance structures such as linear nanometer, rodlike, flower-shaped, tubulose and sea urchin shape, such as: Lee's magnitude
After people's (application number: CN201410377082.1) mixes a certain amount of zinc solution and alkali source and have been prepared for big
Porous materials cuttlebone is put into reaction kettle clock and obtains the uniform nanometer threadiness oxidation of diameter degree after held for some time at a certain temperature
Zinc;Ye Changhui et al. (application number: CN200510094806.2) discloses a kind of single crystal zinc oxide nanometer yarn array/poly crystal aluminium lining
Bottom complex and preparation method thereof;Smelting silver equality people (application number: CN201010606346.8) discloses a kind of nano flower-like oxygen
Change the preparation method of zinc;Zhu Ziqiang et al. (application number: CN200610117564.9) discloses a kind of using hydrothermally synthesizing series
The method of flower shape zinc oxide micrometer/nanometer structure;Xu Junqing et al. (application number: CN201410012786.9), which discloses one kind, to be had
The Zinc oxide catalytic and preparation method thereof of sequence layer structure, SDS are template, and zinc nitrate hexahydrate is zinc source, and sodium hydroxide is
Alkali source carries out the hydro-thermal method preparation of Zinc oxide powder;Yue Hongyan et al. (application number: CN201611174173.0) discloses one kind
The method of hydro-thermal method synthesizing zinc oxide nanometer rods, by certain density zinc nitrate solution, sodium hydroxide solution and pregnancy grade tetramine
Solution, which be blended in, obtains zinc oxide nano rod after heat preservation a period of time at 100 DEG C;Dong Hongxing et al. (application number:
CN201310208236.X) certain density zinc nitrate solution is coated in certain material substrate, after calcining 30min at 500 DEG C
It keeps the temperature 8 hours acquisition presomas at a certain temperature in zinc acetate solution, which is calcined at 150 DEG C and is obtained for 24 hours
Obtain three-dimensional flower-shaped zinc oxide;Tang Pinggui etc. (application number: CN201410764240.9) obtains club shaped structure oxygen by precipitation reaction
Change zinc, then so that nanometer rods is gradually transformed into the tubulose multilevel structure presoma being made of nanometer sheet by dissolving regrowth, finally
Presoma is set to decompose to obtain the tubulose multilevel-structure zinc oxide obtained by nano-particles self assemble by high-temperature roasting;Li great Zhi
(application number: CN201410536535.0) discovery, at room temperature by a certain amount of Zn (NO3)2·6H2O is dissolved in 0.01mol/L
Sodium dodecyl sulfate solution in, make nitric acid zinc concentration up to 0.5mol/L, press zinc nitrate and bicarbonate under magnetic stirring
The molar ratio of sodium 1:1 is slowly added to anhydrous sodium bicarbonate, and sufficiently reaction obtains white precipitate, filters, white precipitate is used respectively
High purity water and dehydrated alcohol washing be placed in 50 DEG C of insulating boxs for several times for 24 hours white presoma;Presoma is placed on small magnetic boat
It is interior, it is placed in electric furnace the thermal decomposition 2h at 280 DEG C and obtains finished product.
The zinc oxide of above method synthesis, is the patterns such as linear common nanometer, rodlike, flower-shaped, tubulose and sea urchin shape,
This case synthesizes four-blade propeller shape nano zinc oxide material for the first time.In addition, the nano zinc oxide material synthesized in the above method,
Operation is very cumbersome, need to be most of to synthesize using cuttlebone or silicon wafer etc. as the substrate for synthesizing specific morphology zinc oxide
Method is not all avoided that the higher high-temperature calcination of energy consumption, and also useful glycerol is at high cost as reaction dissolvent.Therefore, develop one
Environmental-friendly, low in cost, the simple unprecedented new pattern of synthesis route nano zinc oxide material, has very high
Challenge.
Hydro-thermal method is also known as solvent-thermal method, refers in special closed reactor, using aqueous solution as reaction system,
By being heated to reaction system, the environment of a high temperature and pressure is generated, accelerates ionic reaction and promotes hydrolysis, in aqueous solution
Or steam flow remakes standby oxide, obtains oxide nano-particles using separation and heat treatment, can make some in room temperature
The very slow thermodynamical reaction of reaction rate realizes fast reaction under hydrothermal conditions under normal pressure.Therefore, the present inventor this is done into
The method and nano zine oxide of a kind of hydrothermal synthesis four-blade propeller shape nano zine oxide are developed in one step research, and this case is thus
It generates.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of hydrothermal synthesis four-blade propeller shape nano zine oxide
Method and nano zine oxide, using generally the least expensive water as solvent, using soluble zinc nitrate as zinc source, with SDS (dodecyl sodium sulfonate
Sodium) as pattern to directed agents, a period of time, one-step synthesis high-purity, monodispersed four leaves spiral shell are kept the temperature within specified temperatures
Revolve paddle shape nano zine oxide.
In order to solve the above technical problems, the technical solution of the invention is as follows:
A kind of method of hydrothermal synthesis four-blade propeller shape nano zine oxide, the specific steps are as follows:
Step 1: under conditions of temperature is 20 DEG C, the Zn (NO of 1.0mmol is weighed respectively3)2·6H2O and 20.0mmol
NaOH in beaker, with graduated cylinder measure 40.0mL deionized water in the beaker, be placed on magnetic stirring apparatus and be stirred until homogeneous
The dodecyl sodium sulfate that 1.0mmol is added after solution continues the mixed liquor to stir 2-3 hour extremely on magnetic stirring apparatus
Solution is uniformly mixed, and obtains uniform solution;
Step 2: above-mentioned solution is transferred in clean reaction kettle, which is placed in 200 DEG C of thermostatic drying chamber
Middle heat preservation is for 24 hours;
Step 3: after reaction, removing reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens
Reaction kettle;
Step 4: the solution in reaction kettle is poured into crystallising dish, stands, precipitating, separation, dehydrated alcohol is used after separation
Washing 3 times is carried out, white four-blade propeller shape zinc oxide nano powder is obtained, powder is placed in 60 DEG C of thermostatic drying chambers and is carried out
It is dry.
Further, further comprising the steps of in step 1: by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with originally
After washing is clean, rinsed 2-3 times with deionized water, dried for standby.
Further, in step 2, the volume of reaction kettle is 50.0mL.
Further, the vane propeller shape zinc oxide nano powder, the angle between blade and axis are 109 °.
A kind of nano zine oxide is prepared by above-described preparation method.
After adopting the above scheme, the invention has the following advantages that
1, the present invention is under specific reaction temperature (200 DEG C), specific reaction time (for 24 hours) and specific material proportion
Completely new four-blade propeller shape zinc oxide appearance structure is synthesized;
2, the present invention all carries out in aqueous solution, and simple process, low in cost, environment protecting and power-saving avoid existing
Energy consumption is high in technology, is conducive to environmental protection;
3, the material purity height of the invention synthesized, crystallinity height, good dispersion, its morphology controllable degree height etc..
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of the resulting nano zine oxide of the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope (SEM) photograph one of the resulting nano zine oxide of the embodiment of the present invention 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of the resulting nano zine oxide of the embodiment of the present invention 2;
Fig. 4 is the scanning electron microscope (SEM) photograph of the resulting nano zine oxide of the embodiment of the present invention 3;
Fig. 5 is the scanning electron microscope (SEM) photograph of the resulting nano zine oxide of the embodiment of the present invention 4;
Fig. 6 is the scanning electron microscope (SEM) photograph of the resulting nano zine oxide of the embodiment of the present invention 5;
Fig. 7 is the scanning electron microscope (SEM) photograph of the resulting nano zine oxide of the embodiment of the present invention 6;
Fig. 8 is the scanning electron microscope (SEM) photograph two of the resulting nano zine oxide of the embodiment of the present invention 1.
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments.Disclosed is a kind of hydro-thermals
The method for synthesizing four-blade propeller shape nano zine oxide, in an embodiment of the present invention reagent used be on the market can be public
It opens and buys.
Embodiment 1
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 200 DEG C of thermostatic drying chamber and is kept the temperature for 24 hours;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.
The X ray diffracting spectrum of gained powder is as shown in Figure 1, scanning electron microscope (SEM) photograph is as shown in Figure 2 and Figure 8 in embodiment 1.Figure
1 X ray diffracting spectrum shows that the resulting Zinc oxide powder purity is high of this method, crystallinity are high;Its scanning electron microscope knot
Fruit shows that the microscopic appearance is as shown in Figure 2 and Figure 8, defines the pattern as four-blade propeller shape, and as shown in Fig. 2, blade and axis
Between angle be 109 °.
Embodiment 2
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 160 DEG C of thermostatic drying chamber and is kept the temperature for 24 hours;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.The scanning electron microscopy of 2 sample of embodiment
Mirror result is as shown in Figure 3.
Embodiment 3
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 180 DEG C of thermostatic drying chamber and is kept the temperature for 24 hours;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.The scanning electron microscopy of 3 sample of embodiment
Mirror result is as shown in Figure 4.
Embodiment 4
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 220 DEG C of thermostatic drying chamber and is kept the temperature for 24 hours;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.The scanning electron microscopy of 4 sample of embodiment
Mirror result is as shown in Figure 5.
Embodiment 5
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 180 DEG C of thermostatic drying chamber and keeps the temperature 36h;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.The scanning electron microscopy of 5 sample of embodiment
Mirror result is as shown in Figure 6.
Embodiment 6
It by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, is rinsed 2-3 times, is done with deionized water
It is dry stand-by.Under conditions of temperature is 20 DEG C, 1.0mmol (0.2975g) Zn (NO is weighed with assay balance respectively3)2·6H2O、
20.0mmol (0.8g) NaOH measures 40.0mL deionized water in the beaker in beaker, with graduated cylinder, is placed in magnetic stirring apparatus
1.0mmol (0.2724g) SDS (dodecyl sodium sulfate) is added after being stirred until homogeneous solution with suitable rotational speed, by the mixed liquor
Continue 2-3 hour of stirring to solution on magnetic stirring apparatus to be uniformly mixed, obtains uniform solution;Above-mentioned solution is transferred to
Clean volume is in the reaction kettle of 50.0mL;The reaction kettle is placed in 180 DEG C of thermostatic drying chamber and keeps the temperature 48h;Reaction knot
Shu Hou removes reaction kettle from thermostatic drying chamber, after being cooled to room temperature with tap water, opens reaction kettle, is taken out liner;It will
Solution in its liner pours into crystallising dish, stand, precipitating, separation, after separation with dehydrated alcohol carry out washing 3 acquisitions it is white
Powder is placed in 60 DEG C of thermostatic drying chambers and is dried by color zinc oxide nano powder.The scanning electron microscopy of 6 sample of embodiment
Mirror result is as shown in Figure 7.
Above 6 embodiments are compared, are in identical proportion and reaction time difference in embodiment 1,2,3 and 4
Reaction temperature under the different zinc oxide patterns that synthesize.Scanning electron microscope is the results show that reaction temperature produces difference to pattern
The influence of degree, when reaction temperature is 200 DEG C, the pattern of synthesis is four-blade propeller shape, under the conditions of other temperature
Synthesis it is certain it is needle-shaped, rodlike and nanometer is linear, and disperse and it is uneven.Embodiment 3,5 and 6 be in identical reaction temperature and
Match the different zinc oxide patterns synthesized under the different reaction time.Scanning electron microscope different reaction time synthesis as the result is shown
Zinc oxide microstructure difference it is larger, nanowire shape and lath-shaped is presented, and pattern dispersion is uneven.Therefore embodiment 2-6
Sharp contrast is formed with embodiment 1, demonstrating the four-blade propeller shape zinc oxide structures synthesized in embodiment 1 can only be specific
It is synthesized under reaction temperature, specific reaction time and specific material proportion.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore the changes or modifications that claim under this invention and specification are done in every case, it all should belong to the range that the invention patent covers
Within.
Claims (5)
1. a kind of method of hydrothermal synthesis four-blade propeller shape nano zine oxide, it is characterised in that: specific step is as follows: step
One: under conditions of temperature is 20 DEG C, weighing the Zn (NO of 1.0mmol respectively3)2·6H2The NaOH of O and 20.0mmol is in beaker
In, 40.0mL deionized water is measured in the beaker with graduated cylinder, is placed on magnetic stirring apparatus after being stirred until homogeneous solution and is added
The mixed liquor is continued to stir 2-3 hour on magnetic stirring apparatus to solution mixing by the dodecyl sodium sulfate of 1.0mmol
It is even, obtain uniform solution;Step 2: above-mentioned solution is transferred in clean reaction kettle, which is placed in 200 DEG C
It is kept the temperature for 24 hours in thermostatic drying chamber;Step 3: after reaction, removing reaction kettle from thermostatic drying chamber, with being originally water-cooled to
After room temperature, reaction kettle is opened;Step 4: the solution in reaction kettle is poured into crystallising dish, is stood, precipitating, separation, after separation
Washing 3 times is carried out with dehydrated alcohol, white four-blade propeller shape zinc oxide nano powder is obtained, powder is placed in 60 DEG C of constant temperature and is done
It is dried in dry case.
2. a kind of method of hydrothermal synthesis four-blade propeller shape nano zine oxide according to claim 1, it is characterised in that:
It is further comprising the steps of in step 1: by beaker, medicine spoon, graduated cylinder and magnetic agitation rotor with after tap water wash clean, to spend
Ionized water rinses 2-3 times, dried for standby.
3. a kind of method of hydrothermal synthesis four-blade propeller shape nano zine oxide according to claim 1, it is characterised in that:
In step 2, the volume of reaction kettle is 50.0mL.
4. a kind of method of hydrothermal synthesis four-blade propeller shape nano zine oxide according to claim 1, it is characterised in that:
The vane propeller shape zinc oxide nano powder, the angle between blade and axis are 109 °.
5. a kind of nano zine oxide, it is characterised in that: the nano zine oxide is by the described in any item preparation sides claim 1-4
Method is prepared.
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CN103721698A (en) * | 2014-01-10 | 2014-04-16 | 中国天辰工程有限公司 | Zinc oxide catalyst of ordered layered structure and preparation method thereof |
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