CN109778129B - Transparent conductive film based on ultrathin metal - Google Patents
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Abstract
The invention discloses a transparent conductive film based on ultrathin metal, which comprises a bottom dielectric layer, an ultrathin metal layer and a top dielectric layer which are arranged from bottom to top in sequence, wherein the ultrathin metal layer is a silver layer, and the chemical compositions of the bottom dielectric layer and the top dielectric layer are MxZn1‑xAnd O, wherein the average surface roughness of the bottom dielectric layer is 0.1-0.3 nm, M is a doping element, M is any one of Mg, In and Gd, x is the mass ratio of the doping amount of M to the total amount of M and Zn, and x = 0.005-0.5. The transparent conductive film has a three-layer structure, and under the premise that the average optical transmittance of 400-800 nm wavelength is not lower than 80% and the sheet resistance of the film is not higher than 7 omega/sq, the stability in many aspects such as high temperature stability, damp and hot stability, chemical stability, stability in air, scratch resistance stability and the like is greatly improved compared with the existing common transparent conductive film with the same structure, and the application requirements of a plurality of flexible photoelectric devices can be met.
Description
Technical Field
The invention belongs to the field of flexible photoelectric films, and particularly relates to a transparent conductive film based on ultrathin metal.
Background
In recent years, for the demand of wearable devices, thin film photoelectric devices are gradually developing towards flexibility, and the demand of flexible transparent conductive films is increasingly invaluable. At present, a relatively common transparent conductive film in the market is an Indium Tin Oxide (ITO) film, and the requirement of a flexible photoelectric device is difficult to meet due to the limitation of the fragility of an oxide. Therefore, the flexible transparent conductive film product capable of replacing ITO is necessary to be a basic material of future flexible photoelectric products, and is a strategic material of the flexible photoelectric products.
In the flexible transparent conductive film materials which are researched more at present, the metal nanowire film has larger surface roughness; the preparation method of the grid pattern of the metal grid film is complex and has higher cost; the large-area uniform preparation of the graphene and carbon nanotube conductive materials is difficult; the conductivity of organic polymers represented by PEDOT PSS cannot meet the use requirement of high-performance flexible photoelectric devices. In comparison, the transparent conductive film based on the ultrathin metal has the advantages of good mechanical flexibility, good conductivity, uniform optical and electrical properties, low cost, large-scale preparation and the like, and is expected to become an ideal material for replacing ITO.
Ultra-thin metal-based transparent conductive films are typically presented in a D/M/D (dielectric/metal/dielectric) structure. The transmittance and resistivity can be optimized by adjusting the thickness of the dielectric layer and the metal layer, respectively. The resistivity mainly depends on the thickness of the metal layer, the transmittance mainly depends on the matching of the refractive indexes between the dielectric layer and the metal layer, and the dielectric layer can improve the adhesion of the metal layer and protect the metal layer. Although the transparent conductive film of D/M/D structure has better photoelectric characteristics, its stability (including stability in air, scratch resistance, high temperature stability, moist heat stability, etc.) is yet to be enhanced. Since the metal layer is generally thin, the metal self-aggregates under heating or even in air, and thus the transmittance and conductivity are reduced, resulting in deterioration of the optical and electrical properties of the film. The two dielectric layers in the D/M/D structure may also be referred to as a top dielectric layer and a bottom dielectric layer, respectively, at different locations relative to the metal layers. Generally, the bottom dielectric layer and the top dielectric layer are usually metal oxide films, the metal layer is usually a silver film, the bottom dielectric layer is mainly used as a growth buffer layer of the silver film, the top dielectric layer is mainly used as a protective layer of the silver film, and the bottom dielectric layer and the top dielectric layer can adjust the optical performance and the electrical performance of the film system, and can also protect the silver film and improve the physical and chemical properties of the film system. At present, 2 wt% Al2O3Doped ZnO (AZO) materials are often used as the bottom and top dielectric layers. However, the DMD film of AZO/Ag/AZO is not ideal in application, and has the series problems of incomplete protection on a silver film, insufficient film bonding force and the like, and is specifically embodied in that: (1) stable resistance to humidity and heatThe performance is poor, and oxygen and water in the outside air easily penetrate through the AZO layer and diffuse to the silver film, so that the oxidation failure of the silver film is caused; (2) the silver film has poor oxidation resistance in the air, and after the silver film is placed in the air for a period of time, the silver film is easy to oxidize and agglomerate, white spots appear on the surface of the film, and the photoelectric property of the film is further influenced; (3) poor thermal stability during high temperature heat treatment; (4) the AZO layer has poor adhesion with the silver film, and the film surface is scratched when touched and rubbed in the carrying process, so that the quality of the film surface is influenced.
Disclosure of Invention
The invention aims to solve the technical problem that aiming at the defects of the prior art, the invention provides the transparent conductive film based on the ultrathin metal, which greatly improves the stability in various aspects such as high-temperature stability, damp-heat stability, chemical stability, stability in air, scratch resistance stability and the like compared with the prior common transparent conductive film with the same structure on the premise of ensuring that the average optical transmittance of the film with the wavelength of 400-800 nm is not lower than 80% and the sheet resistance of the film is not higher than 7 omega/sq, and can meet the application requirements of various flexible photoelectric devices.
The technical scheme adopted by the invention for solving the technical problems is as follows: the utility model provides a transparent conductive film based on ultra-thin metal, includes bottom dielectric layer, ultra-thin metal level and the top dielectric layer that sets gradually from bottom to top, ultra-thin metal level be the silver layer, bottom dielectric layer with the chemical composition of top dielectric layer be MxZn1-xAnd O, wherein the average surface roughness of the bottom dielectric layer is 0.1-0.3 nm, M is a doping element, M is any one of Mg, In and Gd, x is the mass ratio of the doping amount of M to the total amount of M and Zn, and x is 0.005-0.5.
The invention discloses an ultrathin metal-based transparent conductive film which has a three-layer structure, namely a bottom dielectric layer, an ultrathin metal layer and a top dielectric layer, wherein the bottom dielectric layer and the top dielectric layer are both MxZn1-xAnd O, the middle layer is an ultrathin metal layer (namely a silver layer), and the average surface roughness of the bottom dielectric layer is 0.1-0.3 nm. Specifically, in one aspect, the bottom dielectric layer MxZn1-xThe average surface roughness of O is 0.1-0.3 nm, compared with the bottom of the traditional filmThe AZO layer (the average surface roughness is 0.6nm) is low, the lower average surface roughness indicates that the growth base surface of the middle ultrathin metal layer is smoother, metal atoms tend to two-dimensional layered growth rather than three-dimensional island growth, and the metal layer is not easy to agglomerate under the conditions of high temperature and high humidity, so that the high temperature stability and the damp and hot stability of the transparent conductive film with the three-layer structure are improved; on the other hand, when the element M is doped into ZnO, MxZn1-xThe crystallinity of the O film is weakened, so that the stress between the bottom dielectric layer and the ultrathin metal layer, which is caused by lattice constant mismatch, is reduced, and the scratch resistance stability of the transparent conductive film is better.
The transparent conductive film based on the ultrathin metal disclosed by the invention has the advantages that on the premise of ensuring that the average optical transmittance of the film with the wavelength of 400-800 nm is not lower than 80% and the sheet resistance of the film is not higher than 7 omega/sq, the stability in various aspects such as high temperature stability, damp and hot stability, chemical stability, stability in air, scratch resistance stability and the like is greatly improved compared with the existing common transparent conductive film with the same structure, and the application requirements of various flexible photoelectric devices can be met.
Under the doping of different doping elements M, the control of the optimal doping amount of the doping element M in ZnO, namely the control of the optimal x value determines the average surface roughness of the bottom dielectric layer and the comprehensive stability of the transparent conductive film with the three-layer structure to achieve the optimal effect. Preferably, M is Mg and is added to ZnO in the form of MgO to obtain said MxZn1-xO, x ═ 0.24. Alternatively, preferably, M is In and M is In2O3Is doped into ZnO to obtain the MxZn1-xO, x ═ 0.06. Alternatively, preferably, M is Gd and M is Gd2O3Is doped into ZnO to obtain the MxZn1-xO，x＝0.01。
If the bottom dielectric layer and the top dielectric layer are too thick or too thin, the optical transmittance of the transparent conductive film with the three-layer structure at the visible light wavelength is reduced, so that the thicknesses of the bottom dielectric layer and the top dielectric layer are controlled to be 10-60 nm; if the intermediate metal layer is too thin, the film formation is discontinuous, the resistivity is increased, and if the intermediate metal layer is too thick, the optical transmittance is decreased, so that the thickness of the intermediate metal layer is controlled to be 8-12 nm.
Furthermore, the thicknesses of the bottom dielectric layer and the top dielectric layer are respectively 40nm, and the thickness of the ultrathin metal layer is 10 nm. Under the condition, the optical performance and the electrical performance of the transparent conductive film with the three-layer structure can be optimal.
Preferably, the bottom dielectric layer and the top dielectric layer are both obtained by depositing an oxide target material M at room temperature by radio frequency or medium frequency magnetron sputtering, and the ultrathin metal layer is formed by direct current magnetron sputtering at room temperature. On one hand, magnetron sputtering is suitable for large-area film formation; on the other hand, the film in the application is obtained by sputtering at room temperature, so that the problem that the traditional ITO conductive film needs high-temperature annealing is avoided, and the energy consumption is saved.
Compared with the prior art, the invention has the following advantages: the transparent conductive film based on the ultrathin metal disclosed by the invention has the advantages that on the premise of ensuring that the average optical transmittance of the film with the wavelength of 400-800 nm is not lower than 80% and the sheet resistance of the film is not higher than 7 omega/sq, the stability in various aspects such as high temperature stability, damp and hot stability, chemical stability, stability in air, scratch resistance stability and the like is greatly improved compared with the existing common transparent conductive film with the same structure, and the application requirements of various flexible photoelectric devices can be met.
Drawings
FIG. 1(a) shows a bottom dielectric layer In example 10.06Zn0.94An atomic force micrograph of O, fig. 1(b) is an atomic force micrograph of the bottom AZO layer of a conventional AZO film;
FIG. 2(a) shows In example 1 under the same conditions0.06Zn0.94O/Ag/In0.06Zn0.94An X-ray diffraction phase structure diagram of the O film, and a diagram (b) of an X-ray diffraction phase structure diagram of a common AZO/Ag/AZO film under the same conditions;
FIG. 3 shows a conventional AZO/Ag/AZO thin film and In of example 10.06Zn0.94O/Ag/In0.06Zn0.94O film at wavelength of 400-800 nmAn optical transmittance map;
FIG. 4 shows a conventional AZO/Ag/AZO thin film and In of example 10.06Zn0.94O/Ag/In0.06Zn0.94Placing the O film in an initial state under the conditions of 121 ℃, 97% RH and 0.1Mpa of damp heat experiment for 12 hours, 24 hours and 48 hours respectively, and then amplifying the O film by 1000 times under a fluorescence microscope;
FIG. 5 shows a conventional AZO/Ag/AZO thin film and Mg in example 20.24Zn0.76O/Ag/Mg0.24Zn0.76An optical transmittance diagram of the O film at a wavelength of 400-800 nm;
FIG. 6 shows a conventional AZO/Ag/AZO thin film and Mg in example 20.24Zn0.76O/Ag/Mg0.24Zn0.76Placing the O film in an initial state under the conditions of 121 ℃, 97% RH and 0.1Mpa of damp heat experiment for 12 hours, 24 hours and 48 hours respectively, and then amplifying the O film by 1000 times under a fluorescence microscope;
FIG. 7 shows a conventional AZO/Ag/AZO thin film and Gd in example 30.01Zn0.99O/Ag/Gd0.01Zn0.99An optical transmittance of the O film at a wavelength of 400 to 800 nm.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The ultra-thin metal-based transparent conductive film of embodiment 1, comprising a bottom dielectric layer, an ultra-thin metal layer and a top dielectric layer sequentially arranged from bottom to top, wherein the ultra-thin metal layer is a silver layer, and the top dielectric layer and the bottom dielectric layer both have a chemical composition of InxZn1-xO, wherein In is a doping element, and In is In2O3Is doped into ZnO to obtain InxZn1-xO，x＝0.06。
In example 1, the thickness of the bottom dielectric layer and the top dielectric layer were both 40nm, and the thickness of the ultra-thin metal layer was 10 nm.
In example 1, both the bottom dielectric layer and the top dielectric layer were doped with In2O3The ZnO target material is obtained by radio frequency magnetron sputtering deposition at room temperature, and the specific process comprises the following steps: vacuum degree of less than 6.8 × 10 in background-4In the state of Pa, atPerforming radio frequency magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 100W and the sputtering rate is 4nm/min, wherein the temperature of the substrate is room temperature in the sputtering film formation process. The film of the ultrathin metal layer is formed by direct current magnetron sputtering at room temperature, and the specific process comprises the following steps: vacuum degree of less than 6.8 × 10 in background-4And in the state of Pa, performing direct-current magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 40W and the sputtering rate is 0.34nm/s, wherein the temperature of the substrate is room temperature in the sputtering film formation process.
In example 1, the bottom dielectric layer In0.06Zn0.94An atomic force micrograph of O is shown in FIG. 1 (a). An atomic force micrograph of the bottom AZO layer of a conventional AZO film is shown in fig. 1 (b). As can be seen, the bottom dielectric layer In0.06Zn0.94The average surface roughness of O was 0.25nm and the average surface roughness of the bottom AZO layer of the commonly used AZO film was 0.60 nm. Thus, the bottom dielectric layer In0.06Zn0.94The surface roughness of O is lower than that of an AZO layer at the bottom of a traditional common film, the lower surface roughness indicates that a growth base plane of a middle metal layer (namely a silver layer) is smoother, and metal atoms tend to two-dimensional layered growth rather than three-dimensional island growth, so that the metal layer is not easy to agglomerate under the conditions of high temperature and high humidity, and the high temperature stability and the damp and hot stability of the transparent conductive film with the three-layer structure are improved.
In example 1 under the same conditions0.06Zn0.94O/Ag/In0.06Zn0.94The X-ray diffraction phase structure diagrams of the O film and the conventional AZO/Ag/AZO film are shown In FIG. 2, wherein FIG. 2(a) corresponds to In0.06Zn0.94O/Ag/In0.06Zn0.94O, FIG. 2(b) corresponds to AZO/Ag/AZO.
Common AZO/Ag/AZO thin films and In example 10.06Zn0.94O/Ag/In0.06Zn0.94The optical transmittance of the O film at a wavelength of 400 to 800nm is shown in FIG. 3. It can be seen that the ultra-thin metal-based transparent conductive film of example 1 has an average transmittance of 85% in the visible wavelength range. The sheet resistance of the ultra-thin metal-based transparent conductive film of example 1 was examined to be 5.5 Ω/sq.
FIG. 4 shows a conventional AZO/Ag/AZO thin film and In of example 10.06Zn0.94O/Ag/In0.06Zn0.94The O film was placed in the initial state under the conditions of the moist heat test at 121 ℃, 97% RH and 0.1MPa for 12 hours, 24 hours and 48 hours, respectively, and then magnified 1000 times under a fluorescence microscope. It can be seen that the ultra-thin metal-based transparent conductive film of example 1 is not degraded and degraded when placed under the wet heat test conditions of 121 ℃, 97RH, and 0.1Mpa for 24 hours, as compared to the conventional AZO/Ag/AZO film which is degraded when placed under the same conditions.
The ultra-thin metal-based transparent conductive film of example 1 was annealed at 600 ℃ for 10 minutes in a high temperature furnace without degradation failure, and the conventional AZO/Ag/AZO film had been damaged and failed under the same conditions.
The transparent conductive film based on the ultrathin metal in example 1 was repeatedly brushed 3000 times in a scrub resistant instrument for building materials (brush (5N) + ethanol solution), the film surface was intact without scratches and falling, and under the same conditions, the conventional common AZO/Ag/AZO film had already been scratched and fallen significantly 1000 times.
The ultra-thin metal-based transparent conductive film of embodiment 2 comprises a bottom dielectric layer, an ultra-thin metal layer and a top dielectric layer sequentially arranged from bottom to top, wherein the ultra-thin metal layer is a silver layer, and the top dielectric layer and the bottom dielectric layer both have a chemical composition of MgxZn1-xO, wherein Mg is a doping element, and is doped into ZnO in the form of MgO to obtain MgxZn1-xO，x＝0.24。
In example 2, the thickness of both the bottom dielectric layer and the top dielectric layer was 40 nm; the thickness of the ultra-thin metal layer is 10 nm.
In example 2, the bottom dielectric layer and the top dielectric layer are both obtained by rf magnetron sputtering deposition of a MgO-doped ZnO target at room temperature, and the specific process is as follows: vacuum degree of less than 6.8 × 10 in background-4And in the state of Pa, performing radio frequency magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 100W and the sputtering rate is 1.6nm/min, wherein the temperature of the substrate is room temperature in the sputtering film formation process. The film of the ultrathin metal layer is formed by direct current magnetron sputtering at room temperature, and the specific process comprises the following steps: at background vacuumDegree less than 6.8 multiplied by 10-4And in the state of Pa, performing direct-current magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 40W and the sputtering rate is 0.34nm/s, wherein the temperature of the substrate is room temperature in the sputtering film formation process.
It was examined that in example 2, the bottom dielectric layer Mg0.24Zn0.76The average surface roughness of O was 0.2 nm.
FIG. 5 shows a conventional AZO/Ag/AZO thin film and Mg in example 20.24Zn0.76O/Ag/Mg0.24Zn0.76An optical transmittance of the O film at a wavelength of 400 to 800 nm. It can be seen that the ultra-thin metal-based transparent conductive film of example 2 has an average transmittance of 80% in the visible wavelength range. The sheet resistance of the ultra-thin metal-based transparent conductive film of example 2 was examined to be 6.2 Ω/sq.
FIG. 6 shows a conventional AZO/Ag/AZO thin film and Mg in example 20.24Zn0.76O/Ag/Mg0.24Zn0.76The O film was placed in the initial state under the conditions of the moist heat test at 121 ℃, 97% RH and 0.1MPa for 12 hours, 24 hours and 48 hours, respectively, and then magnified 1000 times under a fluorescence microscope. It can be seen that the ultra-thin metal-based transparent conductive film of example 2 is not degraded and degraded when placed under the wet heat test conditions of 121 ℃, 97RH, and 0.1Mpa for 24 hours, as compared to the conventional AZO/Ag/AZO film which is degraded when placed under the same conditions.
The ultra-thin metal-based transparent conductive film of embodiment 3, comprising a bottom dielectric layer, an ultra-thin metal layer and a top dielectric layer sequentially arranged from bottom to top, wherein the ultra-thin metal layer is a silver layer, and the top dielectric layer and the bottom dielectric layer both have Gd chemical compositionsxZn1-xO, wherein Gd is a doping element and is doped into ZnO in the form of GdO to obtain GdxZn1-xO，x＝0.01。
In example 3, the thickness of both the bottom dielectric layer and the top dielectric layer was 45 nm; the thickness of the ultrathin metal layer is 8 nm.
In example 3, both the bottom and top dielectric layers were Gd-doped2O3The ZnO target material is obtained by radio frequency magnetron sputtering deposition at room temperature, and the specific process is: vacuum degree of less than 6.8 × 10 in background-4And in the state of Pa, performing radio frequency magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 100W and the sputtering rate is 4.1nm/min, wherein the temperature of the substrate is room temperature in the sputtering film formation process. The film of the ultrathin metal layer is formed by direct current magnetron sputtering at room temperature, and the specific process comprises the following steps: vacuum degree of less than 6.8 × 10 in background-4And in the state of Pa, performing direct-current magnetron sputtering film formation under the conditions that the sputtering air pressure is 0.1-1.5 Pa, the sputtering power is 40W and the sputtering rate is 0.34nm/s, wherein the temperature of the substrate is room temperature in the sputtering film formation process.
In example 3, Gd was detected as the bottom dielectric layer0.01Zn0.99The average surface roughness of O was 0.15 nm.
FIG. 7 shows a conventional AZO/Ag/AZO thin film and Gd in example 30.01Zn0.99O/Ag/Gd0.01Zn0.99An optical transmittance of the O film at a wavelength of 400 to 800 nm. It can be seen that the ultra-thin metal-based transparent conductive film of example 3 has an average transmittance of 82% in the visible wavelength range. The sheet resistance of the ultra-thin metal-based transparent conductive film of example 3 was examined to be 6.1 Ω/sq.
The ultra-thin metal-based transparent conductive film of example 3 was left for 24 hours under the hydrothermal test conditions of 121 ℃, 97RH, and 0.1Mpa, and no degradation and failure occurred, as in the case of the conventional AZO/Ag/AZO film, which had failed and degraded.
In conclusion, the performances of the transparent conductive film based on the ultrathin metal, such as high-temperature stability, damp-heat stability, scratch resistance stability and the like, are superior to those of the conventional common AZO/Ag/AZO film.
Claims (5)
1. The utility model provides a transparent conductive film based on ultra-thin metal, includes bottom dielectric layer, ultra-thin metal layer and the top dielectric layer that sets gradually from bottom to top, its characterized in that: the ultrathin metal layer is a silver layer, and the chemical compositions of the bottom dielectric layer and the top dielectric layer are both MxZn1-xO, wherein the average surface roughness of the bottom dielectric layer is 0.1-0.3 nm, M is a doping element,m is any one of Mg, In and Gd, x is the mass ratio of the doping amount of M to the total amount of M and Zn, and x = 0.005-0.5; the bottom dielectric layer and the top dielectric layer are both obtained by the deposition of an oxide target material M through radio frequency or medium frequency magnetron sputtering at room temperature, and the ultrathin metal layer is formed into a film through direct current magnetron sputtering at room temperature; the thickness of the bottom dielectric layer and the thickness of the top dielectric layer are both 10-60 nm, and the thickness of the ultrathin metal layer is 8-12 nm.
2. The ultra-thin metal-based transparent conductive film of claim 1, wherein: m is Mg, and M is doped into ZnO in the form of MgO to obtain the MxZn1-xO，x=0.24。
3. The ultra-thin metal-based transparent conductive film of claim 1, wherein: m is In, M is In2O3Is doped into ZnO to obtain the MxZn1-xO，x=0.06。
4. The ultra-thin metal-based transparent conductive film of claim 1, wherein: m is Gd and M is Gd2O3Is doped into ZnO to obtain the MxZn1-xO，x=0.01。
5. The ultra-thin metal-based transparent conductive film of claim 1, wherein: the thickness of the bottom dielectric layer and the thickness of the top dielectric layer are respectively 40nm, and the thickness of the ultrathin metal layer is 10 nm.
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