Method for preparing zinc oxide electronic film at low temperature

A technology of electronic thin film and zinc oxide, which is applied in the direction of liquid chemical plating, metal material coating technology, coating, etc., can solve the problems of difficult to realize large-scale film formation, strong toxicity of diethyl zinc, easy fire and explosion, etc. Achieve the effect of improving photoelectric conversion efficiency, low cost and good uniformity

Active Publication Date: 2014-04-30
重庆鼎旺科技有限公司
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Problems solved by technology

Another example: Yoshino Kenji. Low-Temperature Growth of ZnO Films by Spray Pyrolysi: Japan, Japanese Journal of Applied Physics, 50(4), (2011) reported that diethyl zinc was used as a raw material, although at a lower temperature (100 ℃) to prepare ZnO film, but the raw material diethyl zinc is highly toxic, easy to catch fire and explode, and expensive; the preparation process is closer to the chemical vapor transport (CVD) method, the process control is relatively complicated, and the control of oxygen and water vapor is strict, so It needs to be carried out under an inert atmosphere; in addition, it is difficult to achieve large-area film formation with a fixed heating table as a heating source

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  • Method for preparing zinc oxide electronic film at low temperature
  • Method for preparing zinc oxide electronic film at low temperature

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Experimental program
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Effect test

Embodiment 1

[0036] A method for preparing ZnO electronic thin film by low-temperature spray pyrolysis, the steps are as follows:

[0037] (1) Precursor preparation

[0038] Dissolve 11g of zinc acetate in deionized water to form a 1mol / L zinc acetate solution, put it in a beaker, and under the action of magnetic force or electric stirring, add concentrated ammonia water dropwise to control the pH of the solution to 8, Zn 2+ Gradually converted to Zn(OH) 2 Precipitation, vacuum filtration, while suction filtration was repeatedly washed with a large amount of deionized water to remove excess anions (CH 3 COO - , NO 3 - , Cl - and other impurities), dry, weigh 5g of precipitate, add 30ml of deionized water and 10ml of methanol, add 10ml of ammonia water, dissolve the precipitate, and form a pH of 11, [(Zn(NH 3 ) 4 ] 2+ A transparent ammonium zinc solution with a concentration of 0.1mol / L was used as a precursor.

[0039] (2) Thin film deposition

[0040] Put the glass fiber reinfor...

Embodiment 2

[0045] A method for preparing ZnO electronic thin film by low temperature spray pyrolysis, same as embodiment 1, wherein:

[0046] In step (1), zinc nitrate is used as the raw material for the preparation of the precursor solution, and 25ml of deionized water and 15ml of methanol are added to the precipitate.

[0047] In step (2), the heating temperature of the substrate is 150°C.

[0048] In step (3), the prepared ZnO thin film and substrate are heated to 250° C., kept for 2 hours, and then cooled naturally.

[0049] The prepared ZnO thin film: the average transmittance in the visible light range reaches more than 85%, the surface roughness is less than 10nm, and does not contain residual solvents, the impurity content is less than 1%, the C axis is preferentially oriented, and the average particle size of the microscopic particles is about 10nm ~20nm, good uniformity.

Embodiment 3

[0051] A method for preparing ZnO electronic thin film by low temperature spray pyrolysis, same as embodiment 1, wherein:

[0052] In step (2), adjust the distance between the nozzle and the substrate to 200mm, take 30ml of the precursor solution into the conical flask, connect the peristaltic pump to the nozzle, control the flow rate of the precursor solution to 0.5ml / min, and adjust the air pressure through the pressure regulating valve. The control is 2atm, and the deposition time is 30min.

[0053] The prepared ZnO thin film: the average transmittance in the visible light range reaches more than 85%, the surface roughness is less than 10nm, and does not contain residual solvents, the impurity content is less than 1%, the C axis is preferentially oriented, and the average particle size of the microscopic particles is about 10nm ~20nm, good uniformity.

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Abstract

The invention provides a method for preparing a zinc oxide electronic film at low temperature, which adopts a spray thermal decomposition process. The method comprises the following steps: precursor solution preparation and film deposition. The method is characterized in that the precursor solution is a [(Zn(NH3)4](OH)2 solution. By using the alkaline [(Zn(NH3)4](OH)2 solution as the precursor solution and a movable heating platform as a heating source and adopting the spray thermal decomposition process, the method can prepare the ZnO film with excellent crystallinity at 130 DEG C or so, has the advantages of no damage on the substrate, low cost, no pollution, no toxicity or harm and simple technique, and can implement large-area film preparation. The substrate material in the technique has wider selection range and small limits; and if a flexible organic film is used as the substrate, a special conveyor can be utilized to implement roll-to-roll production.

Description

technical field [0001] The invention belongs to the preparation of oxide thin films, in particular to a method for preparing zinc oxide (ZnO) electronic thin films by a spray pyrolysis method. Background technique [0002] ZnO film is a multifunctional electronic film, which can be prepared into a transparent conductive oxide film (TCO) by doping B, Al, In, Ga and other elements, and can be used in touch display, solar cell window, low-emissivity (Low-E) glass, etc. has wide application. Recently, it has been found that undoped ZnO thin films have a very important application in the cathode buffer layer of organic solar cells, which can improve their photoelectric conversion efficiency (PCE) and service life. [0003] At present, the key difficulty in the flexibility of organic solar cells lies in the preparation of flexible transparent electrodes and large-area buffer layers. The heat resistance of organic substrates (PET or PMMA) and photosensitive layer films is generall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/12
CPCC23C18/1216C23C18/1258
Inventor 程江张洪涛王祺杨鑫柳红东
Owner 重庆鼎旺科技有限公司
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