CN106430287B - A kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis - Google Patents
A kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis Download PDFInfo
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- CN106430287B CN106430287B CN201610835803.8A CN201610835803A CN106430287B CN 106430287 B CN106430287 B CN 106430287B CN 201610835803 A CN201610835803 A CN 201610835803A CN 106430287 B CN106430287 B CN 106430287B
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- C01—INORGANIC CHEMISTRY
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The present invention relates to a kind of method that low-temperature hydrothermal synthesizes three-dimensional dandelion shape zinc oxide, it comprises the following steps：（a）Zinc oxide crystal seed layer is formed in substrate surface；（b）Soluble zinc salt and alkalescent aminated compounds is soluble in water, then add additive thereto and be configured to growth solution；The additive is 1,3 propane diamine, 1,4 butanediamine, 1,6 hexamethylene diamines, monoethanolamine, polyethyleneimine；（c）By step（a）In the substrate formed with zinc oxide crystal seed layer be put into the growth solution, ultrasound makes the zinc oxide crystal seed come off, take out substrate after the zinc oxide crystal seed is grown in the growth solution.The method that the micro-nano Zinc oxide particles of three-dimensional dandelion shape can so be synthesized, and this method is simple, efficient, energy saving, uniform product appearance, high-specific surface area, can on a large scale synthesize, provide effective approach for extensive synthesizing efficient semiconductor light-catalyst.
Description
Technical field
The present invention relates to a kind of synthetic method of zinc oxide, and in particular to a kind of three-dimensional dandelion shape oxygen of low-temperature hydrothermal synthesis
Change the method for zinc.
Background technology
With the increasingly consumption of the traditional energies such as coal, oil, natural gas, the energy and environmental problem become countries in the world today
Faced urgent problem to be solved.Institute's facing challenges are particularly severe in this respect in China, we are enjoying economic rapid growth
While, be equally also faced with Chinese history it is largest, be related to the most wide, problem of environmental pollution of consequence most serious.Cause
We will pay much attention to discarded object, the processing of emission and circular regeneration for this, reduce resource consumption and environmental pollution.
The photocatalysis technology using metal oxide semiconductor as catalyst that developed recently gets up, to we provide one kind
Preferable using energy source and the method curbed environmental pollution.Efficient, energy consumption is low, behaviour because having for Photocatalytic Oxidation With Semiconductors technology
Make gentle, applied widely, the repeatable utilization of simplicity, reaction condition and the outstanding features such as secondary pollution can be reduced, it is dirty in environment
The favor of people is enjoyed in terms of dye improvement.Eliminated using photocatalytic oxidation and the research of degradation of contaminant becomes environmental project
One hot spot in field.At present, photochemical catalyst is with TiO2Use most, TiO2Chemical stability is good, fast light burn into forbidden band is wide
Degree（Eg=3.2 eV）It is larger.The energy gap and TiO of ZnO2It is similar, while have again than TiO2The quantum efficiency and light of higher are urged
Change efficiency, and preparation method compares TiO2Simply.Therefore, the potentiality of ZnO photochemical catalytic oxidations organic pollution are just progressively research
Persons are approved, and the ZnO for synthesizing specific morphology becomes the hot fields for going research.
The content of the invention
A kind of three-dimensional dandelion shape of low-temperature hydrothermal synthesis is provided the invention aims to overcome the deficiencies in the prior art
The method of zinc oxide.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of three-dimensional dandelion shape oxygen of low-temperature hydrothermal synthesis
Change the method for zinc, it comprises the following steps：
（a）Zinc oxide crystal seed layer is formed in substrate surface；
（b）Soluble zinc salt and alkalescent class compound is soluble in water, then add additive thereto and be configured to grow
Solution；The additive is in 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamines, monoethanolamine and polyethyleneimine
The mixture of one or more composition；
（c）By step（a）In the substrate formed with zinc oxide crystal seed layer be put into the growth solution, ultrasound makes the oxygen
Change zinc crystal seed to come off, the zinc oxide crystal seed is grown in the growth solution after taking out substrate.
Optimally, it is further included：
（d）By step（c）Obtained product centrifuges, and is then dried in vacuo.
Further, it is further included：
（e）By step（d）Obtained product is placed in natural cooling after 300 ~ 500 DEG C of insulations.
Optimally, step（c）In, the zinc oxide crystal seed is small in 50 ~ 80 DEG C of productions 0.5 ~ 5 in the growth solution
When.
Optimally, the soluble zinc salt is one or more of compositions in zinc nitrate, zinc sulfate, zinc chloride and zinc acetate
Mixture.
Further, the alkalescent class compound is selected from hexa, polyacrylamide, formamide, ammonium hydroxide
With the mixture of one or more of compositions in hydrazine hydrate.
Further, the concentration of the soluble zinc salt is 0.01 ~ 0.05mol/L, the alkalescent aminated compounds
Concentration is 0.01 ~ 0.05mol/L, and the concentration of the additive is 0.005 ~ 0.05 mol/L.
Optimally, the step（a）In, zinc-containing solution is coated in glass substrate surface, is subsequently placed at 300 ~ 500 DEG C of heat
Reason forms the zinc oxide crystal seed layer.
Further, in the zinc-containing solution one kind in zinc acetate, zinc nitrate, zinc sulfate and zinc chloride of zinc source or
The mixture of several compositions, the solvent are ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butanol and isobutyl
The mixture of one or more of compositions in alcohol.
Further, the step（a）In, using sol evenning machine on the glass substrate zinc-containing solution described in spin coating, turn
Speed is 800 ~ 1500r/min, and spin-coating time is 30 ~ 60s, and the zinc-containing solution concentration is 0.001 ~ 0.01mol/L.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：Low-temperature hydrothermal of the present invention
The method of the three-dimensional dandelion shape zinc oxide of synthesis, makes zinc oxide crystal seed come off, by soluble zinc salt and weak base by using ultrasound
Property aminated compounds is soluble in water is reacted, while adjust pattern using additive, can so synthesize three-dimensional dandelion shape
Micro-nano Zinc oxide particles method, and this method is simple, efficient, energy saving, uniform product appearance, high-specific surface area, can
It is extensive to synthesize, provide effective approach for extensive synthesizing efficient semiconductor light-catalyst；The dandelion shape zinc oxide exists
Application in optical electro-chemistry field of energy conversion shows very bright and clear prospect.
Brief description of the drawings
Attached drawing 1 synthesizes the flow chart of the method for three-dimensional dandelion shape zinc oxide for low-temperature hydrothermal of the present invention；
Attached drawing 2 is the zinc oxide crystal seed SEM figures prepared in embodiment 1；
Attached drawing 3 is the SEM figures of obtained three-dimensional dandelion shape zinc oxide in different embodiments：（a）Embodiment 1,（b）Implement
Example 2,（c）Embodiment 3；
Attached drawing 4 is the XRD spectra of the three-dimensional dandelion shape zinc oxide prepared in embodiment 1.
Embodiment
The method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis of the present invention, it comprises the following steps：（a）In substrate table
Face forms zinc oxide crystal seed layer；（b）Soluble zinc salt and alkalescent class compound is soluble in water, then additive is added thereto
It is configured to growth solution；The additive is selected from 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamines, monoethanolamine and poly- second
The mixture of one or more of compositions in alkene imines；（c）By step（a）In the substrate formed with zinc oxide crystal seed layer be put into institute
State in growth solution, ultrasound makes the zinc oxide crystal seed come off, and makes the zinc oxide crystal seed molten in the growth after taking out substrate
Grown in liquid.
The above method may also include：（d）By step（c）Obtained product centrifuges, then respectively with deionized water and
Washes of absolute alcohol, is then dried in vacuo；（e）By step（d）Obtained product is placed in after 300 ~ 500 DEG C of insulations certainly
On the one hand so cooling, so can remove organic solvent, on the other hand can stablize the zinc oxide crystal form of preparation.Step
（c）In, the zinc oxide crystal seed when 50 ~ 80 DEG C of productions 0.5 ~ 5 are small, realizes the equal of zinc oxide preferably in the growth solution
Even growth.
The soluble zinc salt is preferably one or more of compositions in zinc nitrate, zinc sulfate, zinc chloride and zinc acetate
Mixture.The alkalescent class compound is preferably selected from hexa, polyacrylamide, formamide, ammonium hydroxide and hydration
The mixture of one or more of compositions in hydrazine.The concentration of the soluble zinc salt is preferably 0.01 ~ 0.05mol/L, described weak
The concentration of alkaline aminated compounds is preferably 0.01 ~ 0.05mol/L, and the concentration of the additive is preferably 0.005 ~ 0.05
Mol/L, can so ensure the quality of three-dimensional dandelion shape zinc oxide with the pattern of formation rule；Meanwhile adjusting can be passed through
The concentration of additive adjusts the pattern of final zinc oxide.
The step（a）In, zinc-containing solution preferably is coated in glass substrate surface, is subsequently placed at 300 ~ 500 DEG C of heat treatments
Form the zinc oxide crystal seed layer；In the zinc-containing solution zinc source in zinc acetate, zinc nitrate, zinc sulfate and zinc chloride one
Kind or several compositions mixture, the solvent for ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butanol and
The mixture of one or more of compositions in isobutanol；Using sol evenning machine on the glass substrate zinc-containing solution described in spin coating,
Rotating speed is 800 ~ 1500r/min, and spin-coating time is 30 ~ 60s, and the zinc-containing solution concentration is 0.001 ~ 0.01mol/L, such energy
One layer of fine and close zinc oxide crystal film layer is enough obtained, so as to improve the quality of final products.
The present invention is further described below in conjunction with attached drawing embodiment.
Embodiment 1
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, as shown in Figure 1, including following
Step：
（a）By glass substrate（1cm×3cm）It is cleaned by ultrasonic 10 min with absolute ethyl alcohol and deionized water respectively, and uses nitrogen
Air-blowing is done；With the zinc acetate ethanol solution of sol evenning machine 100 μ L of spin coating on a glass substrate, rotating speed is 1200 r/min, during spin coating
Between be 50s, wherein zinc acetate ethanol solution concentration is 0.005mol/L；By the good substrate of spin coating in Muffle furnace at 350 DEG C of heat
Manage 30 min, you can one layer of fine and close zinc oxide crystal seed film layer is obtained in substrate, as shown in Figure 2.
（b）Zinc nitrate hexahydrate and hexa are matched somebody with somebody with equimolar concentration mixing soluble in water in vial
Growth solution is made（The concentration of zinc nitrate hexahydrate and the concentration of hexa are 0.025mol/L）, then add and add
Add agent（The concentration of 1,3- propane diamine is 0.010 mol/L）；
（c）The substrate for having zinc oxide nano film to modify is placed in prepared growth solution, there is zinc oxide crystal seed
Diagonally downward, 10 min of ultrasound are so that the seed shedding in substrate of glass is dispersed in reaction solution, so at room temperature in face
Substrate is taken out afterwards, scattered seed-bearing growth-promoting media is grown into 2h at 70 DEG C, you can obtains the oxygen containing three-dimensional dandelion shape
Change zinc nanoparticle；
（d）By step（c）In dandelion shape burnett's solution centrifuged with the speed of 3000r/min, obtain lower floor
Zinc oxide precipitate powder, then respectively cleaning purifying, last zinc oxide precipitate are centrifuged with deionized water and absolute ethyl alcohol dissolving
60 DEG C of vacuum drying, you can obtain dry three-dimensional dandelion shape Zinc oxide nanoparticle after purification；
（e）By step（d）In the three-dimensional dandelion shape Zinc oxide nanoparticle that isolates and purifies, be positioned in crucible plus
It is placed in Muffle furnace, is warming up to 350 DEG C with the speed of 5 DEG C/min, keeps the temperature 2h, then natural cooling puts room temperature；Final product
Pattern such as Fig. 3（a）Shown, its XRD spectra is as shown in Figure 4.
Embodiment 2
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
Basically identical in 1, different is only：1, the 3- propane diamine concentration added is 0.015 mol/L, such as Fig. 3（b）It is shown.
Embodiment 3
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
Basically identical in 1, different is only：1, the 3- propane diamine concentration added is 0.020 mol/L, such as Fig. 3（c）It is shown.
Embodiment 4
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
It is basically identical in 1, unlike：Step（a）In, zinc acetate ethanol solution concentration is 0.001mol/L, is existed using sol evenning machine
Spin coating zinc acetate ethanol solution on glass substrate, rotating speed 800r/min, spin-coating time 60s；Step（b）In, in vial
It is middle by zinc nitrate hexahydrate（Concentration is 0.01mol/L）And hexa（Concentration is 0.05mol/L）It is soluble in water
It is hybridly prepared into growth solution.
Embodiment 5
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
It is basically identical in 1, unlike：Step（a）In, zinc acetate ethanol solution concentration is 0.01mol/L, using sol evenning machine in glass
Spin coating zinc acetate ethanol solution on glass substrate, rotating speed 1500r/min, spin-coating time 30s；Step（b）In, in vial
By zinc nitrate hexahydrate（Concentration is 0.05mol/L）And hexa（Concentration is 0.01mol/L）It is soluble in water mixed
Conjunction is configured to growth solution.
Embodiment 6
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
It is basically identical in 1, unlike：Step（e）The middle three-dimensional dandelion shape Zinc oxide nanoparticle that will be isolated and purified, puts
Capping in crucible is placed in Muffle furnace, to be warming up to 300 DEG C with the speed of 5 DEG C/min, keep the temperature 5h.
Embodiment 7
The present invention provides a kind of method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, its preparation process and embodiment
It is basically identical in 1, unlike：Step（e）The middle three-dimensional dandelion shape Zinc oxide nanoparticle that will be isolated and purified, puts
Capping in crucible is placed in Muffle furnace, to be warming up to 500 DEG C with the speed of 5 DEG C/min, keep the temperature 0.5h.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, it is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should be covered by the protection scope of the present invention.
Claims (5)
- A kind of 1. method of the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis, it is characterised in that it comprises the following steps：（a）Zinc-containing solution is coated in glass substrate surface, 300 ~ 500 DEG C of heat treatments is subsequently placed at and forms the zinc oxide crystal seed Layer；（b）Soluble zinc salt and alkalescent class compound is soluble in water, then add additive thereto and be configured to growth solution； The alkalescent class compound in hexa, polyacrylamide, formamide, ammonium hydroxide and hydrazine hydrate one kind or The mixture of several compositions, the soluble zinc salt are one or more of groups in zinc nitrate, zinc sulfate, zinc chloride and zinc acetate Into mixture, the additive be selected from 1,3- propane diamine, Putriscine, 1,6- hexamethylene diamines, monoethanolamine and polyethyleneimine The mixtures of one or more of compositions in amine, the concentration of the soluble zinc salt are 0.01 ~ 0.05mol/L, the alkalescent The concentration of aminated compounds is 0.01 ~ 0.05mol/L, and the concentration of the additive is 0.005 ~ 0.05 mol/L；（c）By step（a）In the substrate formed with zinc oxide crystal seed layer be put into the growth solution, ultrasound makes the zinc oxide Crystal seed comes off, and the zinc oxide crystal seed is given birth in the growth solution when 50 ~ 80 DEG C of growths 0.5 ~ 5 are small after taking out substrate Length.
- 2. the method for the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis according to claim 1, it is characterised in that it is also Including：（d）By step（c）Obtained product centrifuges, and is then dried in vacuo.
- 3. the method for the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis according to claim 2, it is characterised in that it is also Including：（e）By step（d）Obtained product is placed in natural cooling after 300 ~ 500 DEG C of insulations.
- 4. the method for the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis according to claim 1, it is characterised in that：It is described The mixture of one or more of compositions of the zinc source in zinc acetate, zinc nitrate, zinc sulfate and zinc chloride, solvent in zinc-containing solution For the mixing of one or more of compositions in ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butanol and isobutanol Thing.
- 5. the method for the three-dimensional dandelion shape zinc oxide of low-temperature hydrothermal synthesis according to claim 1, it is characterised in that：It is described Step（a）In, using sol evenning machine, zinc-containing solution described in spin coating, rotating speed are 800 ~ 1500r/min on the glass substrate, spin coating Time is 30 ~ 60s, and the zinc-containing solution concentration is 0.001 ~ 0.01mol/L.
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