CN105460970A - Method for urea assisted hydrothermal synthesis of zinc oxide nanosheet - Google Patents
Method for urea assisted hydrothermal synthesis of zinc oxide nanosheet Download PDFInfo
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- CN105460970A CN105460970A CN201510960903.9A CN201510960903A CN105460970A CN 105460970 A CN105460970 A CN 105460970A CN 201510960903 A CN201510960903 A CN 201510960903A CN 105460970 A CN105460970 A CN 105460970A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a method for a urea assisted hydrothermal synthesis of zinc oxide nanosheet. The cheapest water is used as a solvent, the urea as a nonsurfactant is used as a morphology guiding agent, and dissolvable zinc salt is used as a zinc source, so as to synthesize the high-purity monodispersed zinc oxide nanosheet in one step. The method has the advantages of simple process, easiness in operation of equipment and less pollution and is favorable for industrial mass production.
Description
Technical field
The invention belongs to semiconductive luminescent materials preparation field, relate to a kind of method of urea assisted hydrothermal synthesis Zinc oxide nano sheet.
Background technology
Zinc oxide is a kind of semiconductor material, there are excellent physico-chemical property and good optics, biology, chemistry, semi-conductor and mechanical property etc., have application widely in fields such as uvioresistant, fluorescence, sterilization and sterilization, catalyzer, battery electrode, image recording, sensor, surface wave device and wear-resisting antiskids.ZnO Nanocrystal is a kind of wide bandgap semiconductor materials, its forbidden band gap length 3.37eV under room temperature.Because particle size is between 1-100nm, specific grain surface is long-pending sharply to be increased, make zinc oxide nanocrystalline have its surface effects, small-size effect and macro quanta tunnel effects etc. not available for body lumpy material, in magnetic, optical, electrical, susceptibility etc., there is the incomparable property of general zinc oxide product and novelty teabag.But these properties are relevant with its pattern with novelty teabag, such as: on photoluminescence intensity, the optical property of sheet structure is obviously better than bar-shaped and zinc oxide that is flower-like structure; Microspheroidal zinc oxide has very strong fluorescence in visible region; The photocatalytic activity of sector shape zinc oxide is greater than photocatalytic activity of solid double nut shape zinc oxide etc.Therefore, to the microtexture of zinc oxide nanocrystalline, especially pattern carries out regulation and control synthesis, and the nano zine oxide preparing different-shape has most important theories and practical significance.
At present, the zinc oxide nanocrystalline of the different morphologies such as bar-shaped, banded, flower-shaped and sheet that had multiple method successfully to prepare.As, CN200510094806.2 discloses a kind of single crystal zinc oxide nanometer yarn array/poly crystal aluminium liner compound body and preparation method thereof; CN201010606346.8) a kind of preparation method of nanoscale flower-like zinc oxide is disclosed; CN200610117564.9 discloses a kind of method utilizing hydrothermally synthesizing series flower shape zinc oxide micrometer/nanometer structure; CN201410012786.9 discloses Zinc oxide catalytic of a kind of ordered lamellar structure and preparation method thereof, SDS, is template, and zinc nitrate hexahydrate is zinc source, and sodium hydroxide is alkali source, carries out the hydrothermal method preparation of Zinc oxide powder.The preparation of Zinc oxide nano sheet also has report, as: CN201210134789.0 discloses a kind of Room Temperature Solid State synthetic method of sheet zinc oxide nano-powder, the method for raw material, by Room Temperature Solid State griding reaction, obtains the good sheet zinc oxide powder of degree of crystallinity with zinc acetate and sodium hydroxide; CN201110045892.3 discloses a kind of pearly-lustre color and luster zinc oxalate and Zinc oxide powder preparation method, citric acid or Citrate trianion is added in zinc nitrate, PH is regulated separately to get ammonium oxalate solution, by in two kinds of solution instillation reactors, stir, washing, dry and obtain sheet zinc oxalate powder, after calcining there is the sheet zinc oxide powder of pearly-lustre color and luster; CN201510122642.x discloses a kind ofly has Zinc oxide nano sheet film materials of UV-light performance and preparation method thereof, cleaned substrate is placed in the presoma that zinc nitrate hexahydrate solution becomes with dimethyl aminoboron alkyl solution preparation, after reaction, substrate is taken out and to rinse after drying there is the Zinc oxide nano sheet film materials of UV-light performance; CN201010148752.4 discloses a kind of method of synthesizing flaky nano zinc oxide by low-temperature control, select the quaternary microemulsion that nonionogenic tenside alkyl polyoxyethylene ether, hexanaphthene, n-Octanol and aqueous phase form, with zinc acetate and sodium hydroxide for reactant, drip the microemulsion of sodium hydroxide in the microemulsion of zinc acetate, after hydro-thermal reaction, centrifugation, obtain with after acetone, distilled water and absolute ethanol washing; CN103588239A discloses a kind of method of preparing nano zinc oxide by hydro thermal method, and this patent uses water heat transfer route, assists prepared sheet zinc oxide nano material at lignin sulfonate surfactant.CN200810071953.1 discloses a kind of preparation method of sheet zinc oxide, is dispersed in glycerine by Glacial acetic acid zinc and heats, preparation sheet glycerin zinc precursor; By sheet glycerin zinc precursor heat, sheet zinc oxide.
But, sheet zinc oxide nanometer sheet prepared by aforesaid method is be pattern directed agents by tensio-active agent mostly, synthesize ZnO nano-flakes, the agent of alkyl polyoxyethylene ether isoreactivity is used in building-up process, reaction system aftertreatment trouble containing tensio-active agent, and have disadvantageous effect to environment, also have certain methods to use glycerine and make solvent, cost is high.Therefore, develop an environmental friendliness, synthetic route with low cost carrys out a large amount of making ZnO nanometer sheet, still challenging.
Hydrothermal method is also called hydrothermal method, refer in special closed reactor, adopt the aqueous solution as reaction system, by heating reaction system, produce the environment of a High Temperature High Pressure, speeding-up ion reaction and facilitation of hydrolysis reaction, at the aqueous solution or the standby oxide compound of steam flow recasting, obtain oxide nano-particles through separation and thermal treatment again, some thermodynamical reaction that speed of reaction is very slow at normal temperatures and pressures can be made to realize rapid reaction under hydrothermal conditions.The present inventor makes further research this, and develop a kind of method of urea assisted hydrothermal synthesis Zinc oxide nano sheet, this case produces thus.
Summary of the invention
Technical problem to be solved by this invention is a kind of method providing urea assisted hydrothermal synthesis Zinc oxide nano sheet, the most cheap water is utilized to be solvent, using nonsurfactant urea as pattern directed agents, with solubility zinc nitrate for zinc source, one-step synthesis high purity, monodispersed Zinc oxide nano sheet.
For solving the problems of the technologies described above, technical solution of the present invention is:
A method for urea assisted hydrothermal synthesis Zinc oxide nano sheet, concrete steps are as follows:
Step one: be under the condition of 20 DEG C in temperature, a certain amount of soluble zinc salt and a certain amount of alkali is taken in beaker respectively with analytical balance, soluble zinc salt molar range is: 0.5-1.0mmol, alkali molar weight is scope: 5-30mmol, measure 40.0mL deionized water and carry out uniform stirring, add a certain amount of urea again after stirring to it, urea molar range is: 1.0-20.0mmol, be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: above-mentioned solution is transferred in clean reactor;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reaction 24-48 hour;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, at temperature 50-70 DEG C, dry 6-8 hour.
Further, soluble zinc salt is Zn (NO
3)
26H
2o or ZnCl
2.
Further, adopt decomposable pattern directed agents to be urea in reaction, its molar range is: 1.0-20.0mmol.
Further, alkali is NaOH.
Further, in step 2, the reaction times in reactor is: 24-48h.
After adopting such scheme, the present invention has the following advantages:
1. the present invention all carries out in aqueous, and using nonsurfactant urea as pattern directed agents, avoids in prior art and use tensio-active agent to produce hazardous and noxious substances for pattern directed agents, be conducive to environment protection;
2. present method technique is simple, and equipment is easy to operate, is conducive to industrialization scale operation.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 sample;
Fig. 2 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 2 sample;
Fig. 3 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 3 sample;
Fig. 4 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 4 sample;
Fig. 5 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 5 sample;
Fig. 6 is the scanning electron microscope (SEM) photograph one of the embodiment of the present invention 6 sample;
Fig. 7 is the scanning electron microscope (SEM) photograph two of the embodiment of the present invention 6 sample;
Fig. 8 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 8 sample;
Fig. 9 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 9 sample;
Figure 10 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 10 sample;
Figure 11 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 11 sample;
Figure 12 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 12 sample;
Figure 13 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 13 sample.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.The present invention is understood better to make those skilled in the art.Reagent used is in an embodiment of the present invention and can arrives by open purchase on the market.
Embodiment 1:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, under temperature 70 C, dry 6-8 hour.
By gained pressed powder scanning electron microscope (SEM) photograph in embodiment 1, as can be seen from Figure 1, the Zinc oxide nano sheet pattern adopting present method to obtain is irregular, and the mean size of platy shaped particle is 0.5 μ, and mean thickness is 20nm, and length-to-diameter ratio is 25:1.
Embodiment 2:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 1.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, under temperature 70 C, dry 6-8 hour.
The scanning electron microscope (SEM) photograph of embodiment 2 sample as shown in Figure 2.
Embodiment 3:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 5.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, under temperature 70 C, dry 6-8 hour.
The scanning electron microscope (SEM) photograph of embodiment 3 sample as shown in Figure 3.
Embodiment 4:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 10.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, under temperature 70 C, dry 6-8 hour.
The scanning electron microscope (SEM) photograph of embodiment 4 sample as shown in Figure 4.
Embodiment 5:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 20.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, under temperature 70 C, dry 6-8 hour.
The scanning electron microscope (SEM) photograph of embodiment 5 sample as shown in Figure 5.
By above embodiment 1-5 contrast, urea weight range, in 1-20mmol, all has sheet zinc oxide and generates.And by contrast, in a certain threshold values, along with the increase of urea amount, sheet quantity more Multiple Shape is more obvious.
Embodiment 6:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 5.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 6 sample as shown in Figure 6 and Figure 7.
Embodiment 7:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZn (NO with analytical balance respectively
3)
26H
2o and 20.0mmolNaOH, in beaker, measures 40.0mL deionized water and carries out uniform stirring, and (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Embodiment 8:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZnCl with analytical balance respectively
2with 30.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 8 sample as shown in Figure 8.
By embodiment 6-8 contrast, within the scope of the alkali number of 5-30mmol, (wherein, in embodiment 8, zinc source used is ZnCl all can to generate sheet zinc oxide material
2, the NO in the zinc source wherein in experiment discovery reaction process
3-
-and Cl
-its impact of ion pair is little)-.
Embodiment 9:
Step one: be under the condition of 20 DEG C in temperature, take 0.5mmolZnCl with analytical balance respectively
2with 20.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 9 sample as shown in Figure 9.
Embodiment 10:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZnCl with analytical balance respectively
2with 20.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 10 sample as shown in Figure 10.
Embodiment 11:
Step one: be under the condition of 20 DEG C in temperature, take 2.5mmolZnCl with analytical balance respectively
2with 20.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 24 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 11 sample as shown in figure 11.
By embodiment 9-11 contrast, ZnCl
2within the scope of 0.5-2.5mmol, sheet zinc oxide is all had to generate as zinc source.And use Zn (NO in conjunction with preceding embodiment
3)
26H
2o also can generate sheet zinc oxide when doing zinc source.So, as Zn (NO
3)
26H
2o or ZnCl
2do zinc source has sheet zinc oxide to generate within the scope of 0.5-2.5mmol.
Embodiment 12:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZnCl with analytical balance respectively
2with 20.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 36 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 12 sample as shown in figure 12.
Embodiment 13:
Step one: be under the condition of 20 DEG C in temperature, take 1.0mmolZnCl with analytical balance respectively
2with 20.0mmolNaOH in beaker, measure 40.0mL deionized water and carry out uniform stirring, (chemical name is carbonyl diamine, and molecular formula is CO (NH to add 15.0mmol urea to it again after stirring
2)
2), be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: be transferred to by above-mentioned solution in clean reactor, temperature of reaction kettle is 240 DEG C;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reacts 48 hours;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
The scanning electron microscope (SEM) photograph of embodiment 13 sample as shown in figure 13.
By embodiment 12-13 contrast, under temperature of reaction is 240 ° of C, reaction 24-36h all has sheet zinc oxide to generate.
The above is only preferred embodiment of the present invention, not imposes any restrictions technical scope of the present invention, therefore the change in every case done according to claim of the present invention and specification sheets or modification, all should belong within scope that patent of the present invention contains.
Claims (5)
1. a method for urea assisted hydrothermal synthesis Zinc oxide nano sheet, is characterized in that: concrete steps are as follows:
Step one: be under the condition of 20 DEG C in temperature, a certain amount of soluble zinc salt and a certain amount of alkali is taken in beaker respectively with analytical balance, soluble zinc salt molar range is: 0.5-1.0mmol, alkali molar weight is scope: 5-30mmol, measure 40.0mL deionized water and carry out uniform stirring, add a certain amount of urea again after stirring to it, urea molar range is: 1.0-20.0mmol, be stirred under magnetic stirring apparatus effect evenly, obtain a transparent solution;
Step 2: above-mentioned solution is transferred in clean reactor;
Step 3: thermostatic drying chamber reactor being put into 240 DEG C, reaction 24-48 hour;
Step 4: after reaction terminates, take out reactor from thermostatic drying chamber, after being cooled to room temperature with tap water, open reactor, take out inner bag from reactor;
Step 5: the suspension liquid in inner bag is added in centrifuge tube, centrifugation;
Step 6: add dehydrated alcohol in centrifuge tube, ultrasonic 10 minutes, then be separated with whizzer;
Step 7: repeating step 63 times, obtains pressed powder;
Step 8: pressed powder is placed in thermostatic drying chamber, at temperature 50-70 DEG C, dry 6-8 hour.
2. the method for a kind of urea assisted hydrothermal synthesis Zinc oxide nano sheet according to claim 1, is characterized in that: soluble zinc salt is Zn (NO
3)
26H
2o or ZnCl
2.
3. the method for a kind of urea assisted hydrothermal synthesis Zinc oxide nano sheet according to claim 1, is characterized in that: adopt decomposable pattern directed agents to be urea in reaction, its molar range is: 1.0-20.0mmol.
4. the method for a kind of urea assisted hydrothermal synthesis Zinc oxide nano sheet according to claim 1, is characterized in that: alkali is NaOH.
5. the method for a kind of urea assisted hydrothermal synthesis Zinc oxide nano sheet according to claim 1, it is characterized in that: in step 2, the reaction times in reactor is: 24-48h.
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