CN106430287A - Low-temperature hydro-thermal synthesis method for three-dimensional dandelion-shaped zinc oxide - Google Patents

Low-temperature hydro-thermal synthesis method for three-dimensional dandelion-shaped zinc oxide Download PDF

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CN106430287A
CN106430287A CN201610835803.8A CN201610835803A CN106430287A CN 106430287 A CN106430287 A CN 106430287A CN 201610835803 A CN201610835803 A CN 201610835803A CN 106430287 A CN106430287 A CN 106430287A
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zinc oxide
zinc
dimensional
low
herba taraxaci
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CN106430287B (en
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江林
文鹏
孙迎辉
梁志强
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Suzhou University
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

The invention relates to a low-temperature hydro-thermal synthesis method for three-dimensional dandelion-shaped zinc oxide. The method comprises the following steps: (a) forming a zinc oxide crystal seed layer on the surface of a substrate; (b) dissolving soluble zinc salt and weakly alkaline amine compounds into water, and adding additives to prepare a growth solution, wherein the additives are 1,3-propane diamine, 1,4-butanediamine, 1,6-hexamethylenediamine, ethanol amine and polyethyleneimine; and (c) putting the substrate with the zinc oxide crystal seed layer in the step (a) into the growth solution, carrying out ultrasonic treatment to enable zinc oxide crystal seeds to fall off, taking out the substrate, and enabling the zinc oxide crystal seeds to grow in the growth solution. By virtue of the method, three-dimensional dandelion-shaped micro-nano zinc oxide particles can be synthesized; and the method is simple, efficient and energy-saving, products are uniform in shape, have high specific surface areas and can be synthesized on a large scale, and an effective way is provided for large-scale synthesis of efficient semiconductor photocatalysts.

Description

A kind of method of low-temperature hydrothermal synthesis three-dimensional Herba Taraxaci shape zinc oxide
Technical field
The present invention relates to a kind of synthetic method of zinc oxide is and in particular to a kind of low-temperature hydrothermal synthesizes three-dimensional Herba Taraxaci shape oxygen The method changing zinc.
Background technology
With the day by day consumption of the traditional energies such as coal, oil, natural gas, the energy and environmental problem become countries in the world today Faced problem demanding prompt solution.Institute's facing challenges are particularly severe in this respect for China, and we are enjoying economic rapid growth While, be equally also faced with largest on Chinese history, be related to the widest, problem of environmental pollution of consequence most serious.Cause This our garbage to be paid much attention to, the process of emission and circular regeneration, reduce resource consumption and environmental pollution.
The photocatalysis technology with metal oxide semiconductor as catalyst that developed recently gets up, for we providing one kind Preferably utilization of energy and the method curbed environmental pollution.Efficiency high, energy consumption be low, behaviour because having for Photocatalytic Oxidation With Semiconductors technology Make that easy, reaction condition is gentle, applied widely, repeatable using and the outstanding features such as secondary pollution can be reduced, dirty in environment Dye improvement aspect enjoys the favor of people.Application photocatalytic oxidation eliminates and the research of degradation of contaminant has become environmental project One focus in field.At present, photocatalyst is with TiO2Using most, TiO2Chemical stability good, fast light burn into forbidden band width Degree（Eg=3.2 eV）Larger.The energy gap of ZnO and TiO2Similar, have simultaneously again and compare TiO2Higher quantum efficiency and light are urged Change efficiency, and preparation method compares TiO2Simply.Therefore, the potentiality of ZnO photochemical catalytic oxidation organic pollution are being progressively just research Persons are approved, and the ZnO synthesizing specific morphology becomes the hot fields of research.
Content of the invention
The invention aims to overcoming the deficiencies in the prior art and providing a kind of low-temperature hydrothermal synthesis three-dimensional Herba Taraxaci shape The method of zinc oxide.
For reaching above-mentioned purpose, the technical solution used in the present invention is：A kind of low-temperature hydrothermal synthesis three-dimensional Herba Taraxaci shape oxygen The method changing zinc, it comprises the following steps：
（a）Form zinc oxide crystal seed layer in substrate surface；
（b）Will be soluble in water with alkalescence class compound for soluble zinc salt, then be added thereto to additive and be configured to growth solution； Described additive be selected from one of 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamine, ethanolamine and polyethyleneimine or The mixture of several compositions；
（c）By step（a）In be formed with the substrate of zinc oxide crystal seed layer and put in described growth solution, ultrasonic make described zinc oxide Crystal seed comes off, and so that described zinc oxide crystal seed is grown in described growth solution after taking out substrate.
Optimally, it also includes：
（d）By step（c）The product centrifugation obtaining, subsequently carries out being vacuum dried.
Further, it also includes：
（e）By step（d）The product obtaining is placed in natural cooling after 300 ~ 500 DEG C of insulations.
Optimally, step（c）In, it is little that described zinc oxide crystal seed produces 0.5 ~ 5 in 50 ~ 80 DEG C in described growth solution When.
Optimally, described soluble zinc salt is one or more of zinc nitrate, zinc sulfate, zinc chloride and zinc acetate composition Mixture.
Further, described alkalescence class compound is selected from hexamethylenetetramine, polyacrylamide, Methanamide, ammonia Mixture with one or more of hydrazine hydrate composition.
Further, the concentration of described soluble zinc salt is 0.01 ~ 0.05mol/L, described alkalescence aminated compoundss Concentration is 0.01 ~ 0.05mol/L, and the concentration of described additive is 0.005 ~ 0.05 mol/L.
Optimally, described step（a）In, coat zinc-containing solution in glass substrate surface, be subsequently placed at 300 ~ 500 DEG C of heat Reason forms described zinc oxide crystal seed layer.
Further, in described zinc-containing solution zinc source be selected from one of zinc acetate, zinc nitrate, zinc sulfate and zinc chloride or The mixture of several compositions, described solvent is ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butyl alcohol and isobutyl The mixture of one or more of alcohol composition.
Further, described step（a）In, using sol evenning machine on described glass substrate zinc-containing solution described in spin coating, turn Speed is 800 ~ 1500r/min, and spin-coating time is 30 ~ 60s, and described zinc-containing solution concentration is 0.001 ~ 0.01mol/L.
Because technique scheme is used, the present invention compared with prior art has following advantages：Low-temperature hydrothermal of the present invention The method of the three-dimensional Herba Taraxaci shape zinc oxide of synthesis, makes zinc oxide crystal seed come off by using ultrasonic, by soluble zinc salt and weak base Property aminated compoundss are soluble in water is reacted, adjust pattern using additive simultaneously, so can synthesize three-dimensional Herba Taraxaci shape Micro-nano Zinc oxide particles method, and the method simple, efficiently, energy-conservation, uniform product appearance, high-specific surface area, can Synthesize on a large scale, provide effective approach for extensive synthesizing efficient semiconductor light-catalyst；This Herba Taraxaci shape zinc oxide exists Application in Optical Electro-Chemistry field of energy conversion shows very bright and clear prospect.
Brief description
The flow chart that accompanying drawing 1 synthesizes the method for three-dimensional Herba Taraxaci shape zinc oxide for low-temperature hydrothermal of the present invention；
Accompanying drawing 2 is the zinc oxide crystal seed SEM figure of preparation in embodiment 1；
Accompanying drawing 3 is the SEM figure of the three-dimensional Herba Taraxaci shape zinc oxide being obtained in different embodiments：（a）Embodiment 1,（b）Embodiment 2, （c）Embodiment 3；
Accompanying drawing 4 is the XRD spectra of the three-dimensional Herba Taraxaci shape zinc oxide of preparation in embodiment 1.
Specific embodiment
The method of low-temperature hydrothermal synthesis three-dimensional Herba Taraxaci shape zinc oxide of the present invention, it comprises the following steps：（a）In substrate table Face forms zinc oxide crystal seed layer；（b）Will be soluble in water with alkalescence class compound for soluble zinc salt, then it is added thereto to additive It is configured to growth solution；Described additive is selected from 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamine, ethanolamine and poly- second The mixture of one or more of alkene imines composition；（c）By step（a）In be formed with the substrate of zinc oxide crystal seed layer and put into institute State in growth solution, ultrasonic so that described zinc oxide crystal seed is come off, take out substrate after make described zinc oxide crystal seed described growth molten Grow in liquid.
Said method may also include：（d）By step（c）The product centrifugation obtaining, subsequently respectively deionized water and Washes of absolute alcohol, subsequently carries out being vacuum dried；（e）By step（d）The product obtaining be placed in 300 ~ 500 DEG C insulation after from So cool down, so on the one hand can remove organic solvent, the zinc oxide crystal formation that on the other hand can stably prepare.Step （c）In, described zinc oxide crystal seed produces 0.5 ~ 5 hour in 50 ~ 80 DEG C preferably in described growth solution, realizes the equal of zinc oxide Even growth.
Described soluble zinc salt is preferably one or more of zinc nitrate, zinc sulfate, zinc chloride and zinc acetate composition Mixture.Described alkalescence class compound is preferably selected from hexamethylenetetramine, polyacrylamide, Methanamide, ammonia and hydration The mixture of one or more of hydrazine composition.The concentration of described soluble zinc salt is preferably 0.01 ~ 0.05mol/L, described weak The concentration of alkaline aminated compoundss is preferably 0.01 ~ 0.05mol/L, and the concentration of described additive is preferably 0.005 ~ 0.05 Mol/L, the quality that so ensure that three-dimensional Herba Taraxaci shape zinc oxide is with the pattern of formation rule；Meanwhile, can be by adjusting The concentration of additive is adjusting the pattern of final zinc oxide.
Described step（a）In, preferably coat zinc-containing solution in glass substrate surface, be subsequently placed at 300 ~ 500 DEG C of heat treatments Form described zinc oxide crystal seed layer；In described zinc-containing solution, zinc source is selected from zinc acetate, zinc nitrate, zinc sulfate and zinc chloride Kind or several composition mixture, described solvent be ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butyl alcohol and The mixture of one or more of isobutanol composition；Using sol evenning machine on described glass substrate zinc-containing solution described in spin coating, Rotating speed is 800 ~ 1500r/min, and spin-coating time is 30 ~ 60s, and described zinc-containing solution concentration is 0.001 ~ 0.01mol/L, such energy Enough obtain one layer of fine and close zinc oxide crystal film layer, such that it is able to improve the quality of final products.
Below in conjunction with accompanying drawing embodiment, the present invention is further described.
Embodiment 1
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, as shown in figure 1, include following walking Suddenly：
（a）By glass substrate（1cm×3cm）Use dehydrated alcohol and deionized water to be cleaned by ultrasonic 10 min respectively, and blown with nitrogen Dry；With the zinc acetate ethanol solution of sol evenning machine spin coating 100 μ L on a glass substrate, rotating speed is 1200 r/min, and spin-coating time is 50s, wherein zinc acetate ethanol solution concentration are 0.005mol/L；By the good substrate of spin coating in Muffle furnace 350 DEG C of heat treatments 30 Min, you can one layer of fine and close zinc oxide crystal seed thin layer is obtained on substrate, as shown in Figure 2.
（b）By zinc nitrate hexahydrate and hexamethylenetetramine with the mixing soluble in water of equimolar concentration in vial, join Make growth solution（The concentration of the concentration of zinc nitrate hexahydrate and hexamethylenetetramine is 0.025mol/L）, it is subsequently added and add Plus agent（The concentration of 1,3- propane diamine is 0.010 mol/L）；
（c）The substrate having zinc oxide nano film to modify is placed in the growth solution preparing, has zinc oxide crystal seed face to incline Obliquely, ultrasonic 10 min, so that the seed shedding in substrate of glass is dispersed in reaction solution, then will at room temperature Substrate takes out, and seed-bearing growth-promoting media will be disperseed to grow 2h at 70 DEG C, you can obtain the zinc oxide containing three-dimensional Herba Taraxaci shape Nanoparticle；
（d）By step（c）In Herba Taraxaci shape burnett's solution separated with the centrifugation of 3000r/min, obtain lower floor's oxidation Zinc precipitates powder, then deionized water and anhydrous alcohol solution centrifugation cleaning purification respectively, 60 DEG C of last zinc oxide precipitate Vacuum drying, you can obtain three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle after purification is dried；
（e）By step（d）In isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, be positioned in crucible add a cover in In Muffle furnace, it is warmed up to 350 DEG C with the speed of 5 DEG C/min, is incubated 2h, then natural cooling puts room temperature；The pattern of final product As Fig. 3（a）Shown, its XRD spectra is as shown in Figure 4.
Embodiment 2
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, different is only：1, the 3- propane diamine concentration adding is 0.015 mol/L, such as Fig. 3（b）Shown.
Embodiment 3
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, different is only：1, the 3- propane diamine concentration adding is 0.020 mol/L, such as Fig. 3（c）Shown.
Embodiment 4
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, except for the difference that：Step（a）In, zinc acetate ethanol solution concentration is 0.001mol/L, using sol evenning machine in glass Spin coating zinc acetate ethanol solution on substrate, rotating speed is 800r/min, and spin-coating time is 60s；Step（b）In, will in vial Zinc nitrate hexahydrate（Concentration is 0.01mol/L）And hexamethylenetetramine（Concentration is 0.05mol/L）Mixing soluble in water It is configured to growth solution.
Embodiment 5
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, except for the difference that：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 substrate, rotating speed is 1500r/min, and spin-coating time is 30s；Step（b）In, will in vial Zinc nitrate hexahydrate（Concentration is 0.05mol/L）And hexamethylenetetramine（Concentration is 0.01mol/L）Mixing soluble in water It is configured to growth solution.
Embodiment 6
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, except for the difference that：Step（e）Middle will isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, place Add a cover in crucible in Muffle furnace, be warmed up to 300 DEG C with the speed of 5 DEG C/min, be incubated 5h.
Embodiment 7
The method that the present invention provides a kind of three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis, in its preparation process and embodiment 1 Basically identical, except for the difference that：Step（e）Middle will isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, place Add a cover in crucible in Muffle furnace, be warmed up to 500 DEG C with the speed of 5 DEG C/min, be incubated 0.5h.
Above-described embodiment only technology design to illustrate the invention and feature, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and implements according to this, can not be limited the scope of the invention with this, all according to the present invention Equivalence changes or modification that spirit is made, all should be included within the scope of the present invention.

Claims (10)

1. a kind of method of low-temperature hydrothermal synthesis three-dimensional Herba Taraxaci shape zinc oxide is it is characterised in that it comprises the following steps：
（a）Form zinc oxide crystal seed layer in substrate surface；
（b）Will be soluble in water with alkalescence class compound for soluble zinc salt, then be added thereto to additive and be configured to growth solution； Described additive be selected from one of 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamine, ethanolamine and polyethyleneimine or The mixture of several compositions；
（c）By step（a）In be formed with the substrate of zinc oxide crystal seed layer and put in described growth solution, ultrasonic make described zinc oxide Crystal seed comes off, and so that described zinc oxide crystal seed is grown in described growth solution after taking out substrate.
2. low-temperature hydrothermal synthesizes the method for three-dimensional Herba Taraxaci shape zinc oxide it is characterised in that it also wraps according to claim 1 Include：
（d）By step（c）The product centrifugation obtaining, subsequently carries out being vacuum dried.
3. low-temperature hydrothermal synthesizes the method for three-dimensional Herba Taraxaci shape zinc oxide it is characterised in that it also wraps according to claim 2 Include：
（e）By step（d）The product obtaining is placed in natural cooling after 300 ~ 500 DEG C of insulations.
4. according to claim 1 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Step （c）In, described zinc oxide crystal seed produces 0.5 ~ 5 hour in 50 ~ 80 DEG C in described growth solution.
5. according to claim 1 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described can Soluble zinc salt is the mixture of one or more of zinc nitrate, zinc sulfate, zinc chloride and zinc acetate composition.
6. according to claim 5 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described weak Alkaline species compound is selected from one or more of hexamethylenetetramine, polyacrylamide, Methanamide, ammonia and hydrazine hydrate group The mixture becoming.
7. according to claim 6 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described can The concentration of soluble zinc salt is 0.01 ~ 0.05mol/L, and the concentration of described alkalescence aminated compoundss is 0.01 ~ 0.05mol/L, institute The concentration stating additive is 0.005 ~ 0.05 mol/L.
8. according to claim 1 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described step Suddenly（a）In, coat zinc-containing solution in glass substrate surface, be subsequently placed at 300 ~ 500 DEG C of heat treatments and form described zinc oxide crystal seed Layer.
9. according to claim 8 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described contain In zinc solution, zinc source is selected from the mixture of one or more of zinc acetate, zinc nitrate, zinc sulfate and zinc chloride composition, described molten Agent is the mixed of one or more of ethanol, methanol, isopropanol, water, acetone, methyl ether, ethylene glycol, n-butyl alcohol and isobutanol composition Compound.
10. according to claim 8 the three-dimensional Herba Taraxaci shape zinc oxide of low-temperature hydrothermal synthesis method it is characterised in that：Described Step（a）In, using sol evenning machine on described glass substrate zinc-containing solution described in spin coating, rotating speed be 800 ~ 1500r/min, spin coating Time is 30 ~ 60s, and described zinc-containing solution concentration is 0.001 ~ 0.01mol/L.
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