CN111243939A - Method for preparing semiconductor oxide film based on metal powder - Google Patents
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- CN111243939A CN111243939A CN202010040093.6A CN202010040093A CN111243939A CN 111243939 A CN111243939 A CN 111243939A CN 202010040093 A CN202010040093 A CN 202010040093A CN 111243939 A CN111243939 A CN 111243939A
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
A method for preparing a semiconductor metal oxide film based on metal powder is characterized in that: the preparation method comprises two steps of precursor liquid preparation and oxide film preparation, wherein the precursor liquid preparation is specifically to dissolve metal powder in a mixed solution consisting of hydrogen peroxide, ammonia water and deionized water, fully stir and dissolve for 12 hours, and then age for 2-4 hours to prepare the precursor liquid; the preparation of the oxide film is specifically to prepare a wet film on the surface of a substrate by spin coating or spray coating the prepared precursor solution, and prepare the metal oxide film by thermal annealing treatment. The precursor solution is prepared at a lower concentration, and can be placed for more than 10 days without failure; organic solvent is not used, and the effective recovery of the precursor liquid is facilitated; the prepared film has strong bonding capacity with a substrate and few surface defects, the low-concentration precursor solution is effectively utilized to prepare the metal oxide film with excellent uniformity and compactness, and the prepared film has good use stability.
Description
Technical Field
The invention relates to a preparation method of a functional film, in particular to a method for preparing an oxide film by using metal powder.
Background
At present, in organic polymer solar cells, a semiconductor metal oxide thin film as an interface layer has significant advantages over a conductive polymer in terms of preparation cost and device stability, and thus is receiving increasing attention from the industry. The preparation method of the metal oxide interface layer mainly comprises the following steps: (1) an electrodeposition method, (2) a vacuum thermal evaporation method, (3) a hydrothermal method, (4) a water-soluble metal oxide nanoparticle method, and (5) a sol-gel method. Among these methods, the sol-gel method has unique advantages in terms of production cost and uniformity of thin films, and thus has become the mainstream. The sol-gel method is to utilize metal salt as a precursor source of metal oxide, dissolve the metal salt in an organic solvent or water, perform complex hydrolysis and condensation reactions, form a stable transparent sol system in the solution, slowly polymerize the sol among aged colloidal particles to form gel with a three-dimensional network structure, form a film by spin coating or spray coating and the like, and prepare a metal oxide film structure by drying and annealing. However, with the progress of the times, the conventional sol-gel method for preparing metal oxides also exposes many problems: (1) the preparation cost of the colloidal solution is still high, and once the solution is placed for too long time (such as after 2-3 days), the precursor solution gradually loses efficacy, and the service performance of the precursor solution is affected; (2) some organic solvents adopted by the precursor liquid are harmful to human bodies and environment and are not beneficial to recycling; (3) if the concentration of the prepared precursor solution is low, a uniform and compact metal oxide film cannot be prepared. For example, sol-gel processes produce ZnO using a conventional formulation of anhydrous zinc acetate: ethylene glycol methyl ether: ethanolamine =1 g: 10 ml:0.28 ml. Wherein the anhydrous zinc acetate is 100g/59 yuan, the anhydrous ethylene glycol monomethyl ether is 100 ml/299 yuan, and the ethanolamine is 5 ml/58 yuan (both refer to the Allantin reagent for pricing); when the ZnO film prepared by placing the precursor solution for more than 48 hours in the preparation method is applied to an electron transmission layer of an organic photovoltaic device, the performance of the device is obviously reduced compared with the performance of the ZnO film and the device obtained by placing the precursor solution for 2-4 hours. Therefore, the search for a new precursor solution with low preparation cost, environmental protection and excellent stability and the preparation of a semiconductor metal oxide film with excellent performance are effective ways for improving the application of the precursor solution in the field of organic photovoltaic devices.
Disclosure of Invention
The invention aims to provide a method for preparing a metal oxide film with excellent performance based on metal powder.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a semiconductor metal oxide film based on metal powder is characterized in that: the preparation method comprises two steps of precursor liquid preparation and oxide film preparation, wherein the precursor liquid preparation is specifically to dissolve metal powder in a mixed solution consisting of hydrogen peroxide, ammonia water and deionized water, fully stir and dissolve for 12 hours, and then age for 2-4 hours to prepare the precursor liquid; the preparation of the oxide film is specifically to prepare a wet film on the surface of a substrate by spin coating or spray coating the prepared precursor solution, and prepare the metal oxide film by thermal annealing treatment.
Further, the metal powder may be one of Zn, Cu, Mo, and Ag.
Further, the mixed solution is prepared from 25-28% of ammonia water, 30% of hydrogen peroxide and deionized water according to the volume ratio of 0.5-1.5: 0.06-0.95: 0-0.5.
Further, the mass volume ratio of the metal powder to the mixed liquid is about 1.5-20 mg/ml.
Further, the stirring is specifically carried out at the temperature of 17-25 ℃ for 12 hours at the stirring speed of 300-600 rpm.
In the prior art, if the concentration of the precursor solution is low, the situation that the film is not uniformly covered or even cannot be spin-coated often occurs; the colloid particles have poor dispersibility, the solution stability is reduced, holes and even gaps are easy to appear on the surface of the obtained film, the surface roughness of the film is large, and the uniformity and the compactness are poor, so that the film has large residual stress inside, the adhesion capability is reduced, and the electron/hole transmission performance of the prepared device is also reduced. In addition, if the control is not good in the preparation of the precursor solution, the prepared thin film is easy to have large span of the grain size distribution of the metal oxide grains and uneven size, and the uniformity and compactness of the prepared thin film are also affected. In the invention, metal powder such as Zn powder is oxidized by strong oxidizing property of hydrogen peroxide and complexed by ammonia water in mixed solution under the excitation of water to generate [ Zn (NH)3)4](OH)2、Zn(OH)2The complex mixed system formed by the zinc oxide and other colloidal particle components, the colloidal particles grow gradually in the aging process, the dissolving capacity of zinc in the system is enhanced, the conversion rate of converting the zinc into the ZnO is greatly improved, and simultaneously, the conversion rate of converting the zinc into the ZnO is increasedThe dispersibility of each component in the precursor liquid system is enhanced, and the uniformity of final film forming is improved. Complexes and Zn (OH) during annealing2The decomposition is carried out to generate ZnO crystal grains with small grain diameter, and pores left when ZnO with larger grain diameter generated in the aging process is formed are filled, so that the surface of the film is smooth, the roughness is low, and the film with good uniformity and excellent compactness is finally generated. Meanwhile, other salt ions and organic solvents are not introduced in the preparation of the precursor solution, so that the finally prepared film is ensured to contain no impurities, and the film with smooth surface, low roughness, good uniformity and excellent compactness can be prepared by adopting the precursor solution with lower concentration.
Further, the preparation of the oxide film adopts a spin coating mode, specifically, spin coating is carried out for 20-60 s at the rotating speed of 1500-3500 rpm to prepare a wet film, and then annealing is carried out at the temperature of 150-240 ℃ for 20-60 min.
Further, the preparation of the oxide film adopts a spraying mode, specifically, a substrate is fixed on a movable X-Y platform, the spraying speed is set to be 10-25 mm/s, the air pressure speed is set to be 8-12L/min, the flow is 1cm, the spraying period is 2-4 times, a wet film is prepared, and then annealing is carried out at the temperature of 150-240 ℃ for 20-60 min.
A method for preparing a semiconductor metal oxide film based on metal powder is characterized by comprising the following steps:
(1) preparation of precursor solution
Dissolving metal Zn powder in a mixed solution composed of 30% by mass of hydrogen peroxide, 25-28% by mass of ammonia water and deionized water, fully stirring and dissolving at 17-25 ℃ and 500rpm for 12 hours, and aging for 2-4 hours to obtain a precursor solution, wherein the mass-volume ratio of the metal Zn powder to the mixed solution is 1.5-20 mg/ml, and the volume ratio of the ammonia water, the hydrogen peroxide and the deionized water in the mixed solution is 0.5-1.5: 0.06-0.95: 0-0.5; the dissolving method of the Zn powder comprises the following steps: adding weighed zinc powder into the solution for a plurality of times in a small amount for gradual dissolution reaction;
(2) oxide thin film preparation
Specifically, a prepared precursor solution is spin-coated or spray-coated on the surface of a substrate to prepare a wet film, and then annealing is carried out at the temperature of 150-240 ℃ for 20-60 min; wherein the spin coating is performed at 1500-3500 rpm for 20-60 s, the spray coating is performed by fixing the substrate on a movable X-Y platform, the conventional spray method is adopted to set the spray speed to be 10-25 mm/s, the air pressure speed to be 8-12L/min, the flow is 1cm, and the spray cycle is 2-4 times.
The invention is based on the water solvent method to prepare the metal oxide film, which can be a composite film of more than two metal oxides (such as ZnO and TiO)2Composite film of composition CuO and MoO3Composition of composite films, etc.).
The invention has the following technical effects:
(1) the precursor solution is prepared at a lower concentration at normal temperature, the contents of the powdered metal, hydrogen peroxide and ammonia water are low, the precursor solution can be placed for more than 10 days without failure, the cost is low, and the method is favorable for commercial production.
(2) And no organic solvent is used, so that the method is an environment-friendly oxide film preparation process and is beneficial to effective recovery of precursor liquid.
(3) According to the invention, the conversion rate of ZnO generated by Zn powder is high, so that a film prepared by using a precursor solution with a lower concentration at a lower annealing temperature has strong bonding capability with a substrate and few surface defects, the low-concentration precursor solution is effectively utilized to prepare a metal oxide film with excellent uniformity and compactness, the prepared film has good use stability and excellent electron or hole transmission performance, and the film is used for preparing an organic solar cell and effectively improves the efficiency of a device.
Drawings
FIG. 1: FIG. 1 (a) is an atomic force microscope comparison diagram of a ZnO film prepared by the invention and FIG. 1 (b) is an atomic force microscope comparison diagram of a ZnO film prepared by a comparative example and prepared by a traditional method.
FIG. 2: the comparison graph of the device performance of the ZnO film prepared by the invention and the ZnO film prepared by the comparative example and the traditional method is shown.
FIG. 3: MoO prepared by the invention3Atomic force microscopy of thin films.
FIG. 4: based on the MoO of the invention3Performance of the organic photovoltaic device is shown as a hole transport layer.
FIG. 5: graph comparing performance of organic photovoltaic devices based on the present invention with/without CuO as hole transport layer.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.
Example 1
A method for preparing a semiconductor metal oxide film based on metal powder comprises the following steps:
(1) preparation of precursor solution
Weighing metal Zn powder, dissolving the metal Zn powder in a mixed solution consisting of 30% hydrogen peroxide, 25% ammonia water and deionized water, stirring and dissolving a small amount of the metal Zn powder step by step, fully stirring and dissolving the metal Zn powder for 12 hours at 20 ℃ at 500rpm, and aging the solution for 3 hours to prepare a precursor solution, wherein the mass-volume ratio of the metal Zn powder to the deionized water is 15mg/ml, and the volume ratio of the ammonia water to the hydrogen peroxide to the deionized water in the mixed solution is 1.04:0.06: 0.2;
(2) oxide thin film preparation
Specifically, the prepared precursor solution is spin-coated or spray-coated on the surface of a substrate to prepare a wet film, and then annealing is carried out at 200 ℃ for 20 min; wherein the spin coating is performed at a speed of 3000rpm for 30 s.
The preparation method of the zinc oxide film is applied to the preparation of the solar cell:
the solar cell device structure is as follows: ITO/ZnO/PTB7-Th PC71BM/MoO3Ag, preparing ZnO film on the surface of the ITO transparent conductive electrode by adopting the method, and spin-coating PTB7-Th PC on the surface71Sequentially evaporating 8nm MoO on BM active layer3Thin film and 100nm Ag electrode.
Comparative example: the solar cell structure is ITO/ZnO/PTB7-Th PC71BM/MoO3Ag, different from example 1, in which the ZnO thin film was prepared by using an organic solventPreparing a precursor solution by a traditional method for dissolving zinc acetate by using a solvent, wherein the precursor solution is prepared according to the following steps of: ethylene glycol methyl ether: ethanolamine =1 g, 10 ml and 0.28 ml, and the ZnO film is prepared by spin coating under the same process conditions.
In this example 1, atomic force microscopy images of a metallic ZnO film prepared by an aqueous solution method of Zn powder and a metallic ZnO film prepared by a conventional method of dissolving zinc acetate in an organic solvent in a comparative example are shown in fig. 1, and the metallic ZnO film prepared by the present invention has a roughness of 1.05nm, a low surface roughness, a good uniformity, and a dense structure, as shown in fig. 1 (a), and the metallic ZnO film prepared by the conventional method in the comparative example has a roughness of 1.53nm, a high surface roughness, a relatively poor uniformity, and a relatively poor compactness, as shown in fig. 1 (b). When the method of the invention is applied to the preparation of the organic solar cell, the efficiency of the prepared organic solar cell device is superior to that of the organic solar cell prepared by the comparative example, as shown in fig. 2, the device performance taking the invention as an electron transport layer is as follows: the open-circuit voltage is 0.771V, and the short-circuit current density is 18.36mA/cm2The filling factor is 0.64, and the efficiency is 9.06%; while the device performance in the comparative example was: the open-circuit voltage is 0.767V, and the short-circuit current density is 17.30mA/cm2The fill factor was 0.65 and the efficiency was 8.62%. It can be seen that the device performance of this example 1 is better than the control.
Example 2
A method for preparing a semiconductor metal oxide film based on metal powder comprises the following steps:
(1) preparation of precursor solution
Weighing metal Mo powder, dissolving the metal Mo powder in a mixed solution consisting of 30% hydrogen peroxide, 25% ammonia water and deionized water, stirring and dissolving a small amount of Mo powder step by step, fully stirring and dissolving the Mo powder for 12 hours at a speed of 300rpm at 17 ℃, and aging the mixture for 4 hours to prepare a precursor solution, wherein the mass-volume ratio of the Mo metal powder to the mixed solution is 10 mg/ml, and the volume ratio of the ammonia water, the hydrogen peroxide and the deionized water in the mixed solution is 1.5: 0.5: 0.5;
(2) oxide thin film preparation
Specifically, a prepared precursor solution is subjected to spin coating to prepare a wet film on the surface of a substrate, and then annealing is carried out at 240 ℃ for 60 min; wherein the spin coating is performed at 3500rpm for 60 s.
The preparation method of the molybdenum oxide film is applied to the preparation of the solar cell:
the solar cell device structure is as follows: ITO/MoO3The method is adopted to prepare MoO on the surface of the ITO transparent conductive electrode3The film is coated with a PBDB-T-2F and IT-4F active layer in a spin mode on the surface, and then a LiF film with the thickness of 0.8nm and an Al electrode with the thickness of 100nm are evaporated in sequence. The resulting MoO3The morphology of the thin film and the performance of the organic photovoltaic device are shown in fig. 3 and 4, respectively, and it can be seen that the MoO prepared in this example3The surface roughness of the film was 1.48nm, based on the MoO3The device performance of the film as a hole transport layer is as follows: the open-circuit voltage is 0.799V, and the short-circuit current density is 21.667mA/cm2The fill factor was 0.60 and the efficiency was 10.44%.
Example 3
A method for preparing a semiconductor metal oxide film based on metal powder comprises the following steps:
weighing metal Cu powder, dissolving the metal Cu powder in a mixed solution consisting of 30% hydrogen peroxide and 28% ammonia, gradually adding a small amount of Cu powder for many times, stirring and dissolving, fully stirring and dissolving at the speed of 600rpm at 25 ℃ for 12 hours, and aging for 2 hours to prepare a precursor solution, wherein the mass-volume ratio of the Cu metal powder to the mixed solution is about 1.5 mg/ml, and the volume ratio of ammonia to hydrogen peroxide in the mixed solution is 0.5 ml:0.95 ml;
(2) oxide thin film preparation
Specifically, the prepared precursor solution is spin-coated or spray-coated on the surface of a substrate to prepare a wet film, and then the wet film is annealed at 150 ℃ for 30 min; wherein the spin coating is performed at 1500rpm for 20 s.
The preparation method of the copper oxide film is applied to the preparation of the solar cell:
the solar cell device structure is as follows: ITO/CuO/PTB7-Th PC71BM/LiF/Al, preparing a CuO film on the surface of an ITO transparent conductive electrode by adopting the method, and spin-coating PTB7-Th PC on the surface of the CuO film71And sequentially evaporating a LiF film with the thickness of 0.8nm and an Al electrode with the thickness of 100nm on the BM active layer. For comparison, we prepared organic photovoltaic devices without CuO hole layers under the same conditions, and the results are shown in fig. 5. It can be seen that the device performance using CuO of the present invention as a hole transport layer is: the open-circuit voltage is 0.753V, and the short-circuit current density is 13.46mA/cm2The filling factor is 0.50 percent, and the efficiency is 5.06 percent; the device performance of the CuO-free hole transport layer is as follows: the open-circuit voltage is 0.619V, and the short-circuit current density is 10.22mA/cm2The fill factor was 36.5% and the efficiency was 2.31%, it is clear that the addition of a CuO layer is beneficial to the performance of the device.
Claims (7)
1. A method for preparing a semiconductor metal oxide film based on metal powder is characterized in that: the preparation method comprises two steps of precursor liquid preparation and oxide film preparation, wherein the precursor liquid preparation is specifically to dissolve metal powder in a mixed solution consisting of hydrogen peroxide, ammonia water and deionized water, fully stir and dissolve for 12 hours, and then age for 2-4 hours to prepare the precursor liquid; the preparation of the oxide film is specifically to prepare a wet film on the surface of a substrate by spin coating or spray coating the prepared precursor solution, and prepare the metal oxide film by thermal annealing treatment.
2. The method of claim 1, wherein the metal powder-based method comprises: the metal powder may be one of Zn, Cu, Mo, Ag.
3. The method of claim 2, wherein the metal powder-based method comprises: the mixed solution is prepared from 25-28% of ammonia water, 30% of hydrogen peroxide and deionized water according to the volume ratio of 0.5-1.5: 0.06-0.95: 0-0.5.
4. The method of claim 3, wherein the metal powder-based method comprises: the mass volume ratio of the metal powder to the mixed liquid is about 1.5-20 mg/ml.
5. The method of claim 4, wherein the metal powder-based method comprises: the stirring is carried out for 12 hours at the temperature of 17-25 ℃, and the stirring speed is 300-600 rpm.
6. The method of claim 5, wherein the metal powder-based method comprises: the preparation of the oxide film adopts a spin coating mode, specifically, spin coating is carried out for 20-60 s at the rotating speed of 1500-3500 rpm to prepare a wet film, and then annealing is carried out at the temperature of 150-240 ℃ for 20-60 min.
7. A method for preparing a semiconductor metal oxide film based on metal powder is characterized by comprising the following steps:
(1) preparation of precursor solution
Dissolving metal Zn powder into a mixed solution composed of 30% hydrogen peroxide, 25-28% ammonia water and deionized water, fully stirring and dissolving at the speed of 300-600 rpm at 17-25 ℃ for 12 hours, and aging for 2-4 hours to prepare a precursor solution, wherein the mass-volume ratio of the metal Zn powder to the mixed solution is 1.5-20 mg/ml, and the volume ratio of the ammonia water, the hydrogen peroxide and the deionized water in the mixed solution is 0.5-1.5: 0.06-0.95: 0-0.5;
(2) oxide thin film preparation
Specifically, a prepared precursor solution is subjected to spin coating to prepare a wet film on the surface of a substrate, and then annealing is carried out at the temperature of 150-250 ℃ for 20-60 min; wherein the spin coating is performed at 1500-3500 rpm for 20-60 s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113026002A (en) * | 2021-03-03 | 2021-06-25 | 陕西雷翔新材料科技有限公司 | Thin film metal oxide structure and manufacturing method thereof |
| CN114583055A (en) * | 2022-02-18 | 2022-06-03 | 电子科技大学 | Organic photoelectric detector sprayed with MoO3 film and preparation method thereof |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113026002A (en) * | 2021-03-03 | 2021-06-25 | 陕西雷翔新材料科技有限公司 | Thin film metal oxide structure and manufacturing method thereof |
| CN114583055A (en) * | 2022-02-18 | 2022-06-03 | 电子科技大学 | Organic photoelectric detector sprayed with MoO3 film and preparation method thereof |
| CN114583055B (en) * | 2022-02-18 | 2023-09-15 | 电子科技大学 | Organic photoelectric detector sprayed with MoO3 film and preparation method thereof |
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