CN102260046A - Microwave synthesis method of zinc oxide film with oriented nanorod structure - Google Patents
Microwave synthesis method of zinc oxide film with oriented nanorod structure Download PDFInfo
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Abstract
The invention relates to the synthesis of low-dimensional nanomaterial films, and provides a microwave synthesis method of a zinc oxide film with an oriented nanorod structure. The method is characterized in that a microwave-hydrothermal deposition method is adopted, a zinc salt solution with a molar concentration of 1-150 mM and a hexamethylene tetramine solution are used as raw materials, a blank substrate is placed inside a microwave digestion container, then the container is sealed and placed in a microwave digestion instrument, and after the reaction is carried out at 50-180 DEG C for 0-4 hours, natural cooling is carried out so as to realize the oriented growth of a high-crystallinity film composed of ZnO nanorod arrays on the substrate, wherein the diameter of the nanorods is about 50-300 nm. The microwave-hydrothermal method provided by the invention combines the advantages of microwave and hydrothermal methods, improves the film crystallinity, and significantly improves the film quality. The synthesis method has the advantages of short synthesis time, low synthesis temperature and no need for induced hydrothermal deposition of seed crystals; and the grown ZnO film with the nanorod structure has the advantages of uniform micro morphology, good crystallinity and growth direction perpendicular to the substrate, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of low-dimension nano material film, be specifically related to synthetic zinc oxide nano-rod film and the technology of preparing thereof of aligning of a kind of microwave hydrothermal sedimentation.
Background technology
Zinc oxide is a kind of important wide bandgap semiconductor functional materials, can band gap be 3.3eV under the room temperature, exciton bind energy has very strong free exciton transition luminescence up to 60meV at ultraviolet band, adds abundant raw materials, low price, nontoxic to environment, be suitable for the epitaxy of film, have broad application prospects at the information photoelectric field, be the GaN that continues in recent years, another in the world research focus after the GaAs.Because the ZnO nanostructure of high-sequential growth can be made short-wavelength laser and dye-sensitized nano oxide compound sun power electrode in substrate, becomes the focus of various countries scientist research in recent years.Calendar year 2001 Yang Pei east (HuangM.H. particularly; Mao S.; Feick H.; Yan H.Q.; Wu Y.Y.; Kind H.; Weber E.; Russo R.; YangP.D.Science 2001,292,1897) found ZnO nano wire photic Ultra-Violet Laser phenomenon at room temperature after, promoted the research of the ZnO nano wire (rod) of preparation high quality oriented growth on the solid substrate greatly.And professor Wang Zhonglin successfully develops ZnO nano belt (Pan Z.W.; Dai Z.R.; Wang Z.L.Science2001,29,1947), nano-rings (Kong X.Y.; Ding Y.; Yang R.; Wang Z.L.Science 2004,303,1348), caused great concern in international nano material especially.
At present, prepare method gas-liquid-solid (VLS) or chemical Vapor deposition process (the Wang X.D. of adopting that ZnO aligns nano-rod film more; Summers C.J.; Wang Z.L.Nano Letters 2004,4,423), these method apparatus expensive, the condition harshness, complicated operation, preparation temperature height, need the crystal seed induction and deposition, the prepared ZnO nano-rod film that goes out contains more defective, and is unfavorable for the large-area preparation of ZnO nano-rod film.People such as Vayssieres (Vayssieres L.; Keis K.; Hagfeldt A.; Lindquist S.E.Chemistry of Materials 2001,13,4395) use simple hydrothermal method, on different base by hydrolysis Zn (NO
3)
2Prepare ZnO six prismatic arrays.Because the mismatch ratio of substrate such as glass, sapphire and silicon and ZnO is bigger, hydro-thermal reaction is violent relatively in addition.Make that initial reaction stage is difficult for generating the nucleus of rule relatively at substrate surface, thereby influence the pattern of ZnO array.Govender (Govender, K.; Boyle, D.S.; O ' Brien, P.; Binks D.; West D.; Coleman D.Advanced Materials 2002,14,1221) passes through after sputter layer of metal film on the conductive glass again at Zn (Ac)
2With the growth from solution of hexamethylenetetramine, obtain the uniform array of pattern.Chinese patent CN 1763263A adopts crystal seed to induce the hydro-thermal sedimentation, utilizes zinc solution and amine surfactant soln to grow the ZnO nanometer stick array with preferred orientation.Chinese patent CN100360719C adopts crystal pulling method precoating crystal seed in substrate to prepare the nano level ZnO film.But, many shortcomings that aforesaid method all exists: all need crystal seed to induce, increase the complicated operation degree, increase cost, be unfavorable for large-scale industrial production; Growth time is longer, is unfavorable for large-scale industrial production; The ZnO nano-rod film photoelectric properties that grow are relatively poor, also need anneal just can reach the requirement of preparation ultraviolet laser and electrode of solar battery.
Microwave-hydrothermal method has been widely used in the synthetic of molecular sieve etc., have fast, evenly, the synthetic product particle diameter evenly, advantage such as better crystallinity degree, be used in particular for the ultra-thin molecular screen membrane of synthesis of densified.If therefore can utilize microwave-hydrothermal method to prepare semiconductor film, will might significantly reduce the preparation cost of ultraviolet laser and photovoltaic cell electrode, and then obtain large-area applying.The report that is used for synthesis of nano structural semiconductor film at present also seldom yet there are no report especially for the film of synthetic ZnO nanorod structure.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art problems, provide a kind of microwave hydrothermal sedimentation synthetic zinc oxide nano-rod film and the technology of preparing thereof of aligning, adopt the microwave hydrothermal sedimentation, present method has the crystal seed of need not and induces the hydro-thermal deposition, synthesis temperature is low, and equipment is simple, and is easy and simple to handle, need not expensive vacuum device, many advantages such as suitable scale operation.
The microwave synthesis method of a kind of directional nano bar structure zinc-oxide film that the present invention proposes, adopt the microwave hydrothermal sedimentation, described method need not crystal seed and induces the hydro-thermal deposition, with zinc solution and hexamethylenetetramine solution is raw material, with conductive glass, glass, high molecular polymer, various blank substrate such as inorganic non-metallic are deposition substrate, and substrate is put in micro-wave digestion container inside lining inboard, is put in the microwave dissolver after the micro-wave digestion container sealing, than under the low reaction temperatures, in substrate, grow oriented growth, nanometic zinc oxide rod array film arranged in a uniform, its technological process is specific as follows:
(1) with the zinc solution of 1～150mM and 1～150mM hexamethylenetetramine solution by volume 1: behind the 0.5-2 uniform mixing, put into the micro-wave digestion container, the packing volume of control solution in container accounts for container cumulative volume 60～90%;
(2) substrate is put in the micro-wave digestion container;
(3) will put into microwave dissolver after the micro-wave digestion container sealing, select the reaction of temperature controlling mode or pressure control pattern, 50 ℃～180 ℃ of the temperature of the interior liquid of controlled microwave digestion container, or the pressure in the controlled microwave digestion container is at 0.5MPa～4.0MPa, reaction 10s～4h naturally cools to room temperature with the container taking-up after reaction finishes, and falls to remove the liquid in the micro-wave digestion container, in substrate oriented growth go out, the ZnO nano-stick array thin film of better crystallinity degree, the nanometer rod diameter is about 50～300nm.
Described zinc salt is any or multiple in zinc nitrate, zinc chloride, zinc acetate, the zinc sulfate; Described substrate is any in the various blank substrate such as high molecular polymer, glass, pottery, inorganic non-metallic.Described glass is for being coated with the stannic oxide of mixing fluorine at glass surface or mixing the conductive glass of the stannic oxide coating of indium; Described zinc salt is preferably zinc nitrate.It is 2.45GHz that described microwave reaction adopts frequency, and power is the continuously adjustable microwave oven of 0～1600W.
Oriented growth is meant that the ZnO nanometer rod is along growing perpendicular to the direction of substrate surface basically in substrate, has only the nanometer rod of 1-40% to be with the direction of vertical substrate surface＞angle of 0-30 °.
Because the present invention adopts the microwave hydrothermal sedimentation, need not crystal seed and induce the hydro-thermal deposition, products therefrom has fine crystallinity, the synthetic zinc oxide nano-rod film, directional property is good, the degree of crystallinity height, the nanometer rod size is even, diameter range is between 50～300nm, and length is about 1～2 μ m, and density is 1 * 10
8～2.5 * 10
8Root/cm
2Nanometic zinc oxide rod array film can both be synthesized.Adopt conductive glass, glass, high molecular polymer, various blank substrate such as inorganic non-metallic are deposition substrate, need not crystal seed, obtain the good ZnO nano-rod film of all even directional property in surface.This preparation method is at the synthetic zinc oxide nano-rod film that aligns of low temperature in addition, and required equipment is simple, and cost is low, is suitable for the zinc oxide nano-rod film that scale operation aligns.
Description of drawings
Fig. 1 is the experimental installation structural representation.
Among the figure: 1-microwave dissolver, 2-deposition substrate 3-reaction soln, 4-micro-wave digestion container.
Fig. 2 is the x-ray diffraction pattern of resultant zinc oxide directional nano-rod film among the embodiment 1.
Fig. 3 is the vertical view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 1.
Fig. 4 is the sectional view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 1.
Fig. 5 is the room temperature fluorescence spectrum spectrum of resultant zinc oxide directional nano-rod film among the embodiment 1.
Fig. 6 is the x-ray diffraction pattern of resultant zinc oxide directional nano-rod film among the embodiment 2.
Fig. 7 is the vertical view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 2.
Fig. 8 is the x-ray diffraction pattern of resultant zinc oxide directional nano-rod film among the embodiment 3.
Fig. 9 is the vertical view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 3.
Figure 10 is the x-ray diffraction pattern of resultant zinc oxide directional nano-rod film among the embodiment 4.
Figure 11 is the vertical view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 4.
Figure 12 is the x-ray diffraction pattern of resultant zinc oxide directional nano-rod film among the embodiment 5.
Figure 13 is the vertical view of the scanning electronic microscope of resultant zinc oxide directional nano-rod film among the embodiment 5.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail, but it does not limit the defined invention scope of each accessory claim.
Fig. 1 is the experimental installation structural representation, be the synthetic experimental installation that aligns zinc oxide nano-rod film of microwave hydrothermal sedimentation of the present invention, it is a heating source with MARS type high-throughput closed microwave counteract appearance 1, XP1500 type micro-wave digestion container is the hydro-thermal reaction container, with zinc nitrate, zinc chloride, zinc acetate, zinc salts such as zinc sulfate and hexamethylenetetramine are experimental raw, under lower microwave hydrothermal temperature of reaction, in conductive glass, glass, high molecular polymer, grow the evenly good ZnO nano-rod film of directional property of surface on the various blank substrate such as inorganic non-metallic, substrate becomes 0～90 ° of angle with the microwave hydrothermal reaction kettle bottom surface, compactedness is controlled between 60～90%, and heating mode is temperature controlling mode or pressure control pattern.
Embodiment 1: analytically pure zinc nitrate hexahydrate is added in the distilled water, and constantly stir, be configured to Zn
2+Concentration is the clear solution of 100mM, and gained solution is designated as A; Analytically pure hexamethylenetetramine is added in the distilled water, and constantly stir, be configured to the clear solution that hexamethylenetetramine concentration is 100mM, gained solution is designated as B; Behind the A solution and B solution uniform mixing with above-mentioned preparation, pour in the XP1500 type micro-wave digestion container, compactedness is controlled at 75%, simultaneously the conductive glass substrate is put in XP1500 type micro-wave digestion container inside, substrate and XP1500 type micro-wave digestion container bottoms are at an angle of 90, airtight then XP1500 type micro-wave digestion container puts it in the MARS type high-throughput closed microwave counteract appearance; Select temperature controlling mode to react, hydrothermal temperature is controlled at 90 ℃, pressure 0.3～0.6MPa, and the reaction times is controlled at 60min; Reaction naturally cools to room temperature with container after finishing, and film takes out nature and dries, and promptly synthesizes oriented growth in substrate, the ZnO nano-stick array thin film of better crystallinity degree.XP1500 type micro-wave digestion container and MARS type high-throughput closed microwave counteract appearance are produced by U.S. training peace (CEM) company.
The ZnO film of gained with Japanese D/max2500PC x-ray diffractometer analytic sample of science, is found that product is the hexagonal system zincite phase ZnO (Fig. 2) of JCPDS numbering 36-1451; This sample is carried out displaing microstructure observing with FEIQuanta 200FEG field emission scanning electron microscope to product, and film surface presents equally distributed ZnO nanometer rod, and the diameter of these nanometer rod is about 100～200nm, is about 1.1 μ m, and density is 2.5 * 10
8Root/cm
2, nanometer rod is along grow perpendicular to the direction of substrate surface (having only the nanometer rod of 25-30% to be 10-40 ° angle with the direction of vertical substrate surface) basically.This explanation combines microwave-hydrothermal method with hydrothermal method, can need not crystal seed induction and deposition direct growth and go out the ZnO nanometer stick array, improves the crystal property of film simultaneously, significantly improves the quality of film.In addition, this method generated time is short, and synthesis temperature is low, and the nanorod structure ZnO film microscopic appearance of growth is even, crystal property good, near vertical is grown in the substrate direction, is suitable for the suitability for industrialized production of the directed ZnO nano-rod film of low-cost high-efficiency.
Embodiment 2: analytically pure Zinc Sulphate Heptahydrate is added in the distilled water, and constantly stir, be configured to Zn
2+Concentration is the clear solution of 50mM, and gained solution is designated as A; Analytically pure hexamethylenetetramine is added in the distilled water, and constantly stir, be configured to the clear solution that hexamethylenetetramine concentration is 50mM, gained solution is designated as B; Behind the A solution and B solution uniform mixing with above-mentioned preparation, pour in the XP1500 type micro-wave digestion container, compactedness is controlled at 60%, simultaneously the conductive glass substrate is put in XP1500 type micro-wave digestion container inside, substrate becomes 70 ° of angles with XP1500 type micro-wave digestion container bottoms, airtight then XP1500 type micro-wave digestion container puts it in the MARS type high-throughput closed microwave counteract appearance; Select temperature controlling mode to react, hydrothermal temperature is controlled at 120 ℃, pressure 0.3～0.7MPa, and the reaction times is controlled at 30min; Reaction naturally cools to room temperature with container after finishing, and film takes out nature and dries, and promptly synthesizes oriented growth in substrate, the ZnO nano-stick array thin film of better crystallinity degree.
Embodiment 3: analytically pure zinc acetate dihydrate is added in the distilled water, and constantly stir, be configured to Zn
2+Concentration is the clear solution of 150mM, and gained solution is designated as A; Analytically pure hexamethylenetetramine is added in the distilled water, and constantly stir, be configured to the clear solution that hexamethylenetetramine concentration is 150mM, gained solution is designated as B; Behind the A solution and B solution uniform mixing with above-mentioned preparation, pour in the XP1500 type micro-wave digestion container, compactedness is controlled at 90%, simultaneously plastic-substrates is put in XP1500 type micro-wave digestion container inside, substrate becomes 20 ° of angles with XP1500 type micro-wave digestion container bottoms, airtight then XP1500 type micro-wave digestion container puts it in the MARS type high-throughput closed microwave counteract appearance; Select temperature controlling mode to react, hydrothermal temperature is controlled at 180 ℃, pressure 0.7～4MPa, and the reaction times is controlled at 10min; Reaction naturally cools to room temperature with container after finishing, and film takes out nature and dries, and promptly synthesizes oriented growth in substrate, the ZnO nano-stick array thin film of better crystallinity degree.
Embodiment 4: analytically pure zinc nitrate hexahydrate is added in the distilled water, and constantly stir, be configured to Zn
2+Concentration is the clear solution of 20mM, and gained solution is designated as A; Analytically pure hexamethylenetetramine is added in the distilled water, and constantly stir, be configured to the clear solution that hexamethylenetetramine concentration is 20mM, gained solution is designated as B; Behind the A solution and B solution uniform mixing with above-mentioned preparation, pour in the XP1500 type micro-wave digestion container, compactedness is controlled at 90%, XP1500 type micro-wave digestion container inside will be put in simultaneously at the bottom of the silicon wafer-based, substrate becomes 10 ° of angles with XP1500 type micro-wave digestion container bottoms, airtight then XP1500 type micro-wave digestion container puts it in the MARS type high-throughput closed microwave counteract appearance; Select the pressure control pattern to react, the hydro-thermal pressure-controlling is at 0.5MPa, 100～130 ℃ of temperature, and the reaction times is controlled at 2h; Reaction naturally cools to room temperature with container after finishing, and film takes out nature and dries, and promptly synthesizes oriented growth in substrate, the ZnO nano-stick array thin film of better crystallinity degree.
Embodiment 5: analytically pure zinc nitrate hexahydrate is added in the distilled water, and constantly stir, be configured to Zn
2+Concentration is the clear solution of 90mM, and gained solution is designated as A; Analytically pure hexamethylenetetramine is added in the distilled water, and constantly stir, be configured to the clear solution that hexamethylenetetramine concentration is 90mM, gained solution is designated as B; Behind the A solution and B solution uniform mixing with above-mentioned preparation, pour in the XP1500 type micro-wave digestion container, compactedness is controlled at 60%, simultaneously the conductive glass substrate is put in XP1500 type micro-wave digestion container inside, substrate becomes 10 ° of angles with XP1500 type micro-wave digestion container bottoms, airtight then XP1500 type micro-wave digestion container puts it in the MARS type high-throughput closed microwave counteract appearance; Select the pressure control pattern to react, the hydro-thermal pressure-controlling is at 3.0MPa, 130 ℃～180 ℃ of temperature, and the reaction times is controlled at 3h; Reaction naturally cools to room temperature with container after finishing, and film takes out nature and dries, and promptly synthesizes oriented growth in substrate, the ZnO nano-stick array thin film of better crystallinity degree.
The present invention adopts microwave-hydrothermal method in conjunction with microwave and hydrothermal method advantage, improves the crystal property of film, significantly improves the quality of film.Present method generated time is short, synthesis temperature is low, need not crystal seed and induce hydro-thermal deposition, the nanorod structure ZnO film microscopic appearance of growth is even, crystal property good, perpendicular to the growth of substrate direction, is suitable for the suitability for industrialized production of the directed ZnO nano-rod film of low-cost high-efficiency.
Claims (5)
1. the microwave synthesis method of a directional nano bar structure zinc-oxide film, it is characterized in that: adopt the microwave hydrothermal sedimentation, with zinc solution and hexamethylenetetramine solution is raw material, substrate is put in the micro-wave digestion container, be put in the microwave dissolver after the micro-wave digestion container sealing, need not crystal seed and induce, than under the low reaction temperatures, oriented growth goes out nanometic zinc oxide rod array film arranged in a uniform in substrate, and its technological process is specific as follows:
(1) with the zinc solution of 1～150mM and 1～150mM hexamethylenetetramine solution by volume 1: behind the 0.5-2 uniform mixing, put into the micro-wave digestion container, the packing volume of control solution in container accounts for container cumulative volume 60～90%;
(2) substrate is put in the micro-wave digestion container;
(3) will put into microwave dissolver after the micro-wave digestion container sealing, select the reaction of temperature controlling mode or pressure control pattern, 50 ℃～180 ℃ of the temperature of the interior liquid of controlled microwave digestion container, or the pressure in the controlled microwave digestion container is at 0.5MPa～4.0MPa, reaction 10s～4h naturally cools to room temperature with the container taking-up after reaction finishes, and falls to remove the liquid in the micro-wave digestion container, in substrate oriented growth go out, the ZnO nano-stick array thin film of better crystallinity degree, the nanometer rod diameter is about 50～300nm.
2. preparation method as claimed in claim 1 is characterized in that: described zinc salt is any or multiple in zinc nitrate, zinc chloride, zinc acetate, the zinc sulfate;
Described substrate is any in high molecular polymer, glass, the pottery.
3. preparation method as claimed in claim 2 is characterized in that: described glass is for being coated with the stannic oxide of mixing fluorine at glass surface or mixing the conductive glass of the stannic oxide coating of indium; Described zinc salt is a zinc nitrate.
4. preparation method as claimed in claim 1 is characterized in that: it is 2.45GHz that described microwave reaction adopts frequency, and power is the continuously adjustable microwave oven of 0～1600W.
5. preparation method as claimed in claim 1 is characterized in that:
Oriented growth is meant that the ZnO nanometer rod is along growing perpendicular to the direction of substrate surface basically in substrate, has only the nanometer rod of 1-40% to be with the direction of vertical substrate surface＞angle of 0-30 °.
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