CN101560059A - Aluminum-doped zinc oxide film coating and nano-rod array material as well as preparation method thereof - Google Patents
Aluminum-doped zinc oxide film coating and nano-rod array material as well as preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum-doped zinc oxide film coating and nano-rod array material as well as a preparation method thereof. The aluminum-doped zinc oxide film coating and nano-rod array material comprises the components based on the weight percentage: 95-99% of zinc oxide and 1-5% of aluminum-doped quantity. The preparation method adopts a sol-gel method, zinc acetate and aluminium nitrate are added with organic solvent according to the proportion for heating under reflux; the mixed solution is then added with certain quantity of stabilizing agent for water bath heating at certain temperature and added with organic reagents such as absolute ethyl alcohol, methanamide or methanol and the like to prepare sol according to the need; after that, a spin coating method is adopted to form a film, and the aluminum-doped zinc oxide nano film coating material can be obtained by the processes such as drying, pretreating, repeatedly spin coating, annealing, secondary annealing under the atmosphere of hydrogen and nitrogen and the like; then, a hydrothermal method is adopted for preparing highly oriented aluminum-doped zinc oxide nano-rod and array thereof. The invention has high utilization rate of the raw materials, low cost and simplified preparation technique, and can control the performance and the particle size of the material from the molecular design level.
Description
Technical field
The invention belongs to the thin film technique field, relate to a kind of Al-Doped ZnO and film and nano-rod array material and preparation method thereof.
Background technology
The transparent conductive metal oxide film has broad application prospects, and now has been widely used in fields such as flat pannel display, electromagnetic shielding, thermal barrier, gas sensor, solar cell.Representational transparent conductive metal oxide thin-film material mainly contains In
2O
3, SnO
2With ZnO three big systems.
At present, the transparent conductive metal oxide material is widely used is In
2O
3: Sn (ITO) film, it has transmittance height, good conductivity, substrate tack and reaches hardness by force than advantages such as height, and based on commercially producing of magnetron sputtering technique, ito thin film has been widely used in flat-panel display device.But because starting material reserves such as indium are few, poisonous, and cost an arm and a leg, film preparation cost height, poor stability, thus limited its application in practice.
Single-crystal zinc-oxide nano rod array has characteristics such as no crystal boundary, lattice defect are few, specific surface area height, no matter is separately as low-dimensional materials, still is as the constituting body of microdevice, low-dimensional matrix material, all has wide practical use in field of functional materials.The pure ZnO of desirable stoicheiometry shows as isolator, but because the existence of the point defect of ZnO own makes ZnO depart from desirable stoicheiometry, intrinsic ZnO shows the character of n N-type semiconductorN.By mix III family element (B, Al, Ga, In), or the element F of VII family etc. can reduce the resistivity of ZnO film.
After in ZnO film, mixing the Al element, Al-Doped ZnO ZnO:Al (ZAO) transparent conductive film that forms not only has good photoelectric properties, and the stability of film improves greatly, its outstanding advantage is that raw material is easy to get, nontoxic, cheap, be the ideal substitute of ito thin film, have broad application prospects at photoelectric field.The Al-Doped ZnO nanometer stick array has excellent more photoelectric properties than ZnO array, can be widely used in the flat panel display device electrode, sun power electrode, energy-conservation form, gas sensor, piezoelectric device, emission and opto-electronic device.
The method for preparing at present the ZAO film is many, mainly contains methods such as magnetron sputtering method, spray heating decomposition and sol-gel method.Magnetron sputtering method has the sedimentation rate height, be suitable for advantage such as large area film preparation, is the preparation method of high-quality ZAO film commonly used at present, but the investment cost height, complex manufacturing, use expensive target, and the utilization ratio of target low (about 30%), thereby limited its range of application; Spray heating decomposition prepares the ZAO transparent conductive film has certain application in Korea S, India and Spain, but yet there are no relevant report in China; Sol-gel method is the novel method of preparation high-performance particle and film based on hydrolysis-condensation reaction, and its processing unit is simple, and cost is lower, and growth temperature is low, is easy to control thin film composition, can prepare comparatively ideal transparent conductive film at the molecular level controlled doping.
At present, high directed ZnO nanometer stick array is prepared by different chemistry, electrochemistry and physical deposition method, as gas-phase transport and deposition method, template, hydrothermal method etc.In these methods, the gas-phase transport and deposition method need be not suitable for the large-area preparation film than complex apparatus, higher temperature and metal catalyst; Template causes the destruction of subsiding of film and rod easily in the process of removing template, the film of large-area preparation homogeneous also has difficulties.Compare with other method, hydrothermal method equipment is simple, reaction conditions is gentle, cheap, is the Perfected process of large-area preparation One-Dimensional ZnO nanostructure.With Hydrothermal Preparation ZnO nanometer stick array idol report is arranged both at home and abroad, but the report that utilizes this legal system to be equipped with high directed Al-Doped ZnO nanometer stick array is not seen at present.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of Al-Doped ZnO to film and nano-rod array material and preparation method thereof, this nano coating film metrial and high directional nano rod array material are used for the flat panel display device electrode, sun power electrode, energy-conservation form, gas sensor, piezoelectric device, emission and opto-electronic device, the ZAO film of preparation improves more than 5% than similar existing film transmissivity, and resistivity reduces more than 10%.
For achieving the above object, technical scheme of the present invention is:
A kind of Al-Doped ZnO film is characterized in that, its composition according to weight percent content is: zinc oxide 95～99%, aluminium doping are 1～5%, and the diameter of Al-Doped ZnO composite oxides is between 40nm～60nm.
A kind of high directed Al-Doped ZnO nanometer stick array, it is characterized in that its composition according to weight percent content is: zinc oxide 95～99%, aluminium doping are 1～5%, and the diameter of Al-Doped ZnO composite oxides is between 40nm～60nm.
A kind of preparation method of Al-Doped ZnO film is characterized in that, may further comprise the steps:
1) preparation colloidal sol: take by weighing Zinc diacetate dihydrate and nine water aluminum nitrates and be dissolved in and form solution in the organic solvent, make in solution zinc acetate concentration between 0.4～0.7mol/L, the mass ratio of [AL/Zn] is between 1%～5%, solution evaporation is refluxed, heated and stirred, with the ratio adding stablizer of the solution after refluxing, at 55 ℃ of-75 ℃ of heating in water bath in the 0.5%-2% of cumulative volume; Add organic reagent constant volume (organic solvent and organic reagent volume ratio are 13～16: 1, for example 15: 1) again, make colloidal sol, leave standstill again after the concussion and make colloidal sol even, standby; [above ratio 0.4～0.7mol/L and 0.5%-2% are the ratios with respect to cumulative volume, comprise organic reagent.】
2) spin coating plated film: substrate after will cleaning and described colloidal sol are placed on and carry out the spin coating plated film on the desk-top sol evenning machine, adopt the low speed gear of 500-1500r/min rotating speed to drip glue, adopt the even glue of high gear of 1000-5000r/min rotating speed; Make wet film;
3) drying and pre-treatment: the wet film that makes is dry under 75-100 ℃ temperature, to evaporate moisture and a part of organism; Film with dried gained makes the organism in the film volatilize fully under 250-500 ℃ temperature again;
4) annealing: the film that obtains after the pre-treatment is made anneal under 350-700 ℃, naturally cool to room temperature then.
5) atmosphere annealing: under 1%-5% hydrogen and 95%-99% nitrogen atmosphere, under 400-490 ℃ of temperature, film is carried out second annealing and handle, make Al-Doped ZnO film.
Organic solvent in the described step 1) is ethylene glycol monomethyl ether, Virahol; Stablizer is thanomin, methyl ethyl diketone, and organic reagent is dehydrated alcohol or methane amide.
A kind of preparation method of high directional nano rod array is characterized in that, may further comprise the steps,
1) preparation method according to above-mentioned Al-Doped ZnO film makes attached to the Al-Doped ZnO film on the indium tin oxide sheet glass, and promptly nanometer Al-Doped ZnO Seed Layer is standby;
2) with hydrothermal method growing high-oriented nanometer stick array on the nano zine oxide Seed Layer; May further comprise the steps:
A) preparation precursor aqueous solution: take by weighing Zinc diacetate dihydrate and be dissolved in distilled water to make the concentration of Zinc diacetate dihydrate in solution be 0.01～0.05mol/L, in [AL/Zn] mass ratio is that 1%～5% ratio takes by weighing nine water aluminum nitrates and is dissolved in the distilled water, mix above-mentioned two kinds of solution, ratio in 20g/L～35g/L adds hexamethylenetetramine, 0.5%～3% ratio in the mixing solutions cumulative volume adds tensio-active agent polymine or poly maleimide, stir, make precursor aqueous solution;
B) reaction:, put into hydrothermal reaction kettle then with the nanometer Al-Doped ZnO Seed Layer on the distilled water cleaning indium tin oxide sheet glass; In reactor, pour precursor aqueous solution into, sealed reactor; Place vacuum drying oven under 90 ℃ of-95 ℃ of temperature, to carry out hydro-thermal reaction reactor;
C) separation and dry: after reacting the question response still cooling that finishes, take out the indium tin oxide sheet glass, use distilled water flushing, adhere to high directed Al-Doped ZnO nanometer stick array on the indium tin oxide sheet glass at this moment; Isolate reaction soln with whizzer and make high directed Al-Doped ZnO nanometer powder, clean powder with distilled water again; High directed Al-Doped ZnO nanometer stick array will promptly be got after the gained powder for drying.
Beneficial effect of the present invention is as follows:
The present invention adopts Prepared by Sol Gel Method ZAO film, adopts hydrothermal reaction at low temperature to prepare narrow diameter distribution, the high directed ZAO nanometer stick array of crystalline orientation.Compared with prior art, the starting material source is abundant, low price, owing to adopt the nanometer package technique to prepare ZAO film and synthetic ZAO array system, on molecular level, regulate and control synthetic, can improve raw-material utilization ratio, reduce cost, simplify preparation technology, be convenient to stoichiometry control precursor solution, revise composition easily, from the performance and the granularity of the horizontal control material of molecular designing, the ZAO film of preparation improves more than 5% than similar existing film transmissivity, and resistivity reduces more than 1/10th, therefore this film has the transmittance height, and characteristics such as conduct electricity very well.Because in the ZAO film formation process, at first gel-film is through decomposing, a series of processes such as oxidation and solid state reaction form the oxide compound nucleus on substrate, surface diffusion makes nucleus growth form a series of polycrystalline island, the polycrystalline island combines with contiguous island and forms network, just because of having formed this polycrystalline island, make the ZAO film surface to reduce, so film forming good uniformity, to the substrate strong adhesion, and be applicable to large-area plated film and batch process, because starting material are easy to get, and price is cheap more a lot of than indium tin oxide, under lower temperature, from solution, be settled out needed oxide coating in large area in addition, and through being heat-treated to the ZAO film, needing no vacuum equipment, thereby significantly reduced cost of manufacture, simplify technology, can improve utilization rate of raw materials, can be from the performance and the granularity of the horizontal control material of molecular designing.Can be widely used in fields such as laser, an emission, opto-electronic device.
Description of drawings:
Fig. 1: process flow diagram of the present invention.
Embodiment
Embodiment 1: take by weighing Zinc diacetate dihydrate 65.853g, ANN aluminium nitrate nonahydrate 5.418g is dissolved in it fully and is made into 250 ml solns in the organic solvent, and organic solvent can be selected ethylene glycol monomethyl ether for use, evaporation refluxes, heated and stirred adds 3.5 milliliters of stabilizer alcohol amine in the solution after backflow, stirred 1 hour at 60 ℃ of heating in water bath, add the organic reagent dehydrated alcohol again and be settled to 500 milliliters, get transparent homogeneous colloidal sol, collosol concentration 0.6mol/L, doping content [Al/Zn] is 2.0%; Make substrate with slide glass, substrate should clean up, and purging method is for using washing powder and tap water flush away substrate stain; Soak the flush away greasy dirt with the 10%NaOH dilute solution; Soak with potassium bichromate solution; Use deionized water rinsing; Use immersions such as deionized water, formaldehyde solution, ethanol solution, acetone soln more successively respectively, carry out the hertzian wave ultrasonic cleaning after each solution soaking respectively; And 3-5 time repeatedly, the sheet glass after cleaning is placed in dehydrated alcohol or the acetone always stores, in loft drier, use at once after the drying before filming.Utilize the spin coating method film forming, earlier in the following glue of dropleting of 1000r/min rotating speed 15 seconds, then under the 3000r/min rotating speed even glue [technical term was spared glue: promptly on the substrate of high speed rotating in 20 seconds, all kinds of glues that instil utilize centrifugal force to make to drop in on-chip glue to be coated on the substrate equably; Drip glue: promptly with the special-purpose gluing equipment glue that on substrate, instils equably].100 ℃ of dryings 10 minutes; Then 300 ℃ of pre-treatment 10 minutes; Film repeatedly after the cooling [filming repeatedly here do not comprise above-mentioned drying and preprocessing process] 5-10 time; Film was annealed 1 hour at 550 ℃; Finally 450 ℃ of second annealings 1 hour under 5% hydrogen and 95% nitrogen atmosphere, make Al-Doped ZnO nano coating film metrial (as the ZAO Seed Layer of embodiment 3), utilize the transmissivity of photoelectric properties in the visible region of the film sample that this processing parameter prepares to be higher than 50%, resistivity is lower than 5.0 * 10
-3Ω cm.This film sample improves more than 5% than similar existing film transmissivity, and resistivity reduces more than 1/10th.
Embodiment 2: take by weighing Zinc diacetate dihydrate 43.902g, ANN aluminium nitrate nonahydrate 5.586g is dissolved in it fully and is made into 250 ml solns in the organic solvent, and organic solvent can be selected Virahol for use, evaporation refluxes, heated and stirred adds 4.5 milliliters of stablizer methyl ethyl diketones in the solution after backflow, stirred 1 hour at 70 ℃ of heating in water bath, add the organic reagent methane amide again and be settled to 500 milliliters, get transparent homogeneous colloidal sol, collosol concentration 0.4mol/L, doping content [Al/Zn] 3.1%; Make substrate with slide glass, substrate should clean up, and purging method is with embodiment 1.Utilize the spin coating method film forming, earlier, under the 3000r/min rotating speed, spare glue 25 seconds then in the following glue of dropleting of 1000r/min rotating speed 20 seconds.100 ℃ of dryings 10 minutes; Then 300 ℃ of pre-treatment 10 minutes; Film 5-10 time repeatedly after the cooling; Film was annealed 1 hour at 600 ℃; Finally 450 ℃ of second annealings 1 hour under 5% hydrogen and 95% nitrogen atmosphere make Al-Doped ZnO nano coating film metrial (as the ZAO Seed Layer of embodiment 4).Utilize the transmissivity of photoelectric properties in the visible region of the film sample that this processing parameter prepares to be higher than 89%, resistivity is lower than 5.3 * 10
-3Ω cm.
Embodiment 3: the method for employing embodiment 1 prepares Al-Doped ZnO (ZAO) Seed Layer makes it attached on the sheet glass that scribbles indium tin oxide (ITO), take by weighing Zinc diacetate dihydrate 2.195g and ANN aluminium nitrate nonahydrate 0.1806g respectively, be dissolved in the distilled water respectively, two kinds of solution of remix, add the 15g hexamethylenetetramine, add 8 milliliters of tensio-active agent polymines, stir, be settled to 500 milliliters, stir precursor aqueous solution.Clean the ZAO Seed Layer repeatedly with distilled water, tilt to put into hydrothermal reaction kettle then; In reactor, pour precursor aqueous solution into to volumetrical 60%, sealed reactor; Place reactor vacuum drying oven to carry out hydro-thermal reaction for 95 ℃, the reaction times is 6h; After reacting the question response still cooling that finishes, take out the ito glass sheet, wash repeatedly with distilled water; With whizzer separating reaction solution, clean 5 times with distilled water again and get powder; Place 65 ℃ thermostat container dry sheet glass and powder, prepare ZAO nanometer stick array and the powder thereof of diameter in 45-55nm, height C axle orientation.
Embodiment 4: the method for employing embodiment 2 prepares Al-Doped ZnO (ZAO) Seed Layer makes it attached on the sheet glass that scribbles indium tin oxide (ITO); Take by weighing Zinc diacetate dihydrate 5.488g and ANN aluminium nitrate nonahydrate 0.469g respectively, be dissolved in respectively in the distilled water, two kinds of solution of remix, add the 20g hexamethylenetetramine, add 8 milliliters of tensio-active agent poly maleimides, stir, be settled to 500 milliliters, stir precursor aqueous solution.Clean the ZAO Seed Layer repeatedly with distilled water, tilt to put into hydrothermal reaction kettle then; In reactor, pour precursor aqueous solution into to volumetrical 70%, sealed reactor; Place reactor vacuum drying oven to carry out hydro-thermal reaction for 95 ℃, the reaction times is 6h; After reacting the question response still cooling that finishes, take out the ito glass sheet, wash repeatedly with distilled water; Adopt the method separating reaction solution of vacuum filtration, clean 5 times with distilled water again and get powder; Place 65 ℃ thermostat container dry sheet glass and powder, make ZAO nanometer stick array and the powder thereof of diameter in 50-60nm, height C axle orientation.
Embodiment 5: take by weighing Zinc diacetate dihydrate 32.927g, ANN aluminium nitrate nonahydrate 1.128g is dissolved in it fully and is made into 250 ml solns in the organic solvent, and organic solvent can be selected ethylene glycol monomethyl ether for use, evaporation refluxes, heated and stirred adds 5.5 milliliters of stabilizer alcohol amine in the solution after backflow, stirred 1 hour at 70 ℃ of heating in water bath, add the organic reagent dehydrated alcohol again and be settled to 500 milliliters, get transparent homogeneous colloidal sol, collosol concentration 0.3mol/L, doping content [Al/Zn] is 0.62%; Make substrate with slide glass, substrate should clean up, and purging method is with embodiment 1.Utilize the spin coating method film forming, earlier, under the 3000r/min rotating speed, spare glue 20 seconds then in the following glue of dropleting of 1000r/min rotating speed 15 seconds.Drying is 10 minutes under 90 ℃ of temperature; Then 350 ℃ of pre-treatment 10 minutes; Film 5-10 time repeatedly after the cooling; Film was annealed 1 hour at 500 ℃; Finally second annealing 1 hour under 2% hydrogen and 98% nitrogen atmosphere and 400 ℃ of temperature makes the Al-Doped ZnO nano coating film metrial, and the transmissivity of film sample in the visible region of utilizing this processing parameter to prepare is higher than 88%, and resistivity is lower than 5.3 * 10
-3Ω cm.
Embodiment 6: take by weighing Zinc diacetate dihydrate 21.954g, ANN aluminium nitrate nonahydrate 3.613g, it is dissolved in fully is made into 250 ml solns in the organic solvent, organic solvent can be selected Virahol for use, and evaporation refluxes, heated and stirred, add 4.0 milliliters of stablizer methyl ethyl diketones in the solution after backflow, stirred 1 hour, get transparent homogeneous colloidal sol at 55 ℃ of heating in water bath, collosol concentration 0.2mol/L, doping content [Al/Zn] 4.0%; Make substrate with slide glass, substrate should clean up, and purging method is with embodiment 1.Utilize the spin coating method film forming, earlier, under the 3000r/min rotating speed, spare glue 30 seconds then in the following glue of dropleting of 1000r/min rotating speed 25 seconds.100 ℃ of dryings 10 minutes; Then 300 ℃ of pre-treatment 15 minutes; Film 5-10 time repeatedly after the cooling; Film was annealed 1 hour at 450 ℃; Finally 430 ℃ of second annealings 1 hour under 3% hydrogen and 97% nitrogen atmosphere make the Al-Doped ZnO nano coating film metrial.The transmissivity of film sample in the visible region of utilizing this processing parameter to prepare is higher than 88%, and resistivity is lower than 5.4 * 10
-3Ω cm.
Claims (5)
1. an Al-Doped ZnO film is characterized in that, its composition according to weight percent content is: zinc oxide 95～99%, aluminium doping are 1～5%, and the diameter of Al-Doped ZnO composite oxides is between 40nm～60nm.
2. one kind high directed Al-Doped ZnO nanometer stick array, it is characterized in that its composition according to weight percent content is: zinc oxide 95～99%, aluminium doping are 1～5%, and the diameter of Al-Doped ZnO composite oxides is between 40nm～60nm.
3. the preparation method of an Al-Doped ZnO film is characterized in that, may further comprise the steps:
1) preparation colloidal sol: take by weighing Zinc diacetate dihydrate and nine water aluminum nitrates and be dissolved in and form solution in the organic solvent, make in the solution acetic acid zinc concentration between 0.4～0.7mol/L, [AL/Zn] mass ratio is between 1%～5%, solution evaporation is refluxed, heated and stirred, with the ratio adding stablizer of the solution after refluxing, at 55 ℃ of-75 ℃ of heating in water bath in the 0.5%-2% of cumulative volume; Add the organic reagent constant volume again, make colloidal sol, leave standstill again after the concussion and make colloidal sol even, standby;
2) spin coating plated film: substrate after will cleaning and described colloidal sol are placed on and carry out the spin coating plated film on the desk-top sol evenning machine, adopt the low speed gear of 500-1500r/min rotating speed to drip glue, adopt the even glue of high gear of 1000-5000r/min rotating speed; Make wet film;
3) drying and pre-treatment: the wet film that makes is dry under 75-100 ℃ temperature, to evaporate moisture and a part of organism; Film with dried gained makes the organism in the film volatilize fully under 250-500 ℃ temperature again;
4) annealing: the film that obtains after the pre-treatment is made anneal under 350-700 ℃, naturally cool to room temperature then.
5) atmosphere annealing: under 1%-5% hydrogen and 95%-99% nitrogen atmosphere, under 400-490 ℃ of temperature, film is carried out second annealing and handle, make Al-Doped ZnO film.
4, the preparation method of the directed Al-Doped ZnO nanometer stick array of height according to claim 3 is characterized in that, the organic solvent in the described step 1) is ethylene glycol monomethyl ether, Virahol; Stablizer is thanomin, methyl ethyl diketone, and organic reagent is dehydrated alcohol or methane amide.
5. the preparation method of one kind high directional nano rod array is characterized in that, may further comprise the steps,
1) preparation method according to claim 3 or 4 described Al-Doped ZnO films makes attached to the Al-Doped ZnO film on the indium tin oxide sheet glass, and promptly nanometer Al-Doped ZnO Seed Layer is standby;
2) with hydrothermal method growing high-oriented nanometer stick array on the nano zine oxide Seed Layer; May further comprise the steps:
A) preparation precursor aqueous solution: take by weighing Zinc diacetate dihydrate and be dissolved in distilled water to make the concentration of Zinc diacetate dihydrate in solution be 0.01～0.05mol/L, in [AL/Zn] mass ratio is that 1%～5% ratio takes by weighing nine water aluminum nitrates and is dissolved in the distilled water, mix above-mentioned two kinds of solution, ratio in 20g/L～35g/L adds hexamethylenetetramine, 0.5%～3% ratio in the mixing solutions cumulative volume adds tensio-active agent polymine or poly maleimide, stir, make precursor aqueous solution;
B) reaction:, put into hydrothermal reaction kettle then with the nanometer Al-Doped ZnO Seed Layer on the distilled water cleaning indium tin oxide sheet glass; In reactor, pour precursor aqueous solution into, sealed reactor; Place vacuum drying oven under 90 ℃ of-95 ℃ of temperature, to carry out hydro-thermal reaction reactor;
C) separation and dry: after reacting the question response still cooling that finishes, take out the indium tin oxide sheet glass, use distilled water flushing, adhere to high directed Al-Doped ZnO nanometer stick array on the indium tin oxide sheet glass at this moment; Isolate reaction soln with whizzer and make high directed Al-Doped ZnO nanometer powder, clean powder with distilled water again; High directed Al-Doped ZnO nanometer stick array will promptly be got after the gained powder for drying.
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