Ultra-thin silver base thin film, multi-layer composite transparent electric conduction thin film and preparing method and application thereof

A transparent conductive film, multi-layer composite technology, applied in the coating, superimposed layer plating, metal material coating process and other directions, can solve the photoelectric performance island growth mode and aging effect, the oxygen doping concentration is difficult to accurately control, the preparation conditions of the conductive film are harsh and other problems, to achieve the effect of convenient application, good mechanical flexibility, and good mechanical flexibility

Active Publication Date: 2017-10-17
HEBEI UNIVERSITY
7 Cites 10 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0006] One of the objectives of the present invention is to provide an ultra-thin silver-based film to solve the problems of poor electrical properties and difficulty in controlling the oxygen doping concentration of the existing conductive film containing silver oxide
[0007] The second object of the present invention is to provide a method for preparing an ultra-thin silver-based film, to prepare an ultra-thin silver-based film using vacuum coating technology at room temperature, to solve the problem of the harsh preparation conditions of the existin...
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Method used

As can be seen from Table 1, by changing O2/(Ar+O2) flow ratio in Ag(O) deposition process can realize the adjustment of oxygen doping concentration x in Ag(O) film easily, in the table The oxygen doping concentration x of the Ag(O) film was obtained by X-ray photoelectron spectroscopy measurement of a thicker Ag(O) film (50 nm) deposited under the same experimental conditions. Analyzing the data in the table, it can be found that with the increase of x in the Ag(O) film, the average visible light transmittance of the sample shows a trend of first increasing and then decreasing, and the surface resistance of the sample shows a trend of first decreasing and then increasing The tendency is that without changing other experimental conditions, there is a better x, so that the prepared silver-based multilayer composite transparent conductive film has better photoelectric proper...
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Abstract

The invention provides an ultra-thin silver base thin film, a multi-layer composite transparent electric conduction thin film and a preparing method and application thereof. The ultra-thin sliver base thin film is of a double-layer structure and comprises an Ag (O) layer and a continuous ultra-thin Ag layer which is located on and makes contact with the Ag (O) layer; the thickness of the Ag (O) layer is 0.5 nm-5 nm, and the thickness of the Ag layer is 2 nm-10 nm; and the oxygen doping concentration x is greater than or equal to 1% and less than or equal to 24% in the Ag (O) layer. The multi-layer composite transparent electric conduction thin film comprises a base and at least one Ag (O) / Ag double-layer which is located on the base. According to the ultra-thin silver base thin film and the multi-layer composite transparent electric conduction thin film based on the ultra-thin silver base thin film, excessive dependence of the thin film overall electric conduction on the oxygen doping concentration of the Ag (O) layer is weakened to a certain extent, the technical problems of difficult precise controlling over the oxygen doping concentration of the Ag (O) layer and the like are solved, the transparent electric conduction thin film with better mechanical flexibility and composite photoelectricity performance is obtained, preparing in a room temperature condition is achieved, cost is low, and the application prospects are broad.

Application Domain

Vacuum evaporation coatingSputtering coating +2

Technology Topic

Electrically conductiveMaterials science +2

Image

  • Ultra-thin silver base thin film, multi-layer composite transparent electric conduction thin film and preparing method and application thereof
  • Ultra-thin silver base thin film, multi-layer composite transparent electric conduction thin film and preparing method and application thereof
  • Ultra-thin silver base thin film, multi-layer composite transparent electric conduction thin film and preparing method and application thereof

Examples

  • Experimental program(8)
  • Comparison scheme(2)

Example Embodiment

[0062] Example 1
[0063] Such as figure 1 As shown, an ultra-thin silver-based film includes an Ag(O) layer 2 and an Ag layer 3. The Ag(O) layer 2 is located on the substrate 1, and the Ag layer 3 is located on the Ag(O) layer 2 and is in contact with the Ag(O) layer 2. To contact. The total thickness of the Ag(O)/Ag double-layer film is preferably 3 nm to 12 nm, wherein the thickness of the Ag(O) layer 2 is 0.5 to 5 nm, preferably 1 nm to 3 nm. The thickness of the Ag layer 3 is 2 nm-10 nm, preferably 3 nm-7 nm. In the Ag(O) layer 2, the oxygen doping concentration x satisfies 1≤x≤24%, preferably, 2%≤x≤15%.
[0064] The substrate 1 can be a dielectric, semiconductor or metal substrate, including glass, quartz, silicon wafer, stainless steel, etc.; it can also be an organic polymer substrate, including polyethylene terephthalate (PET), polyethylene naphthalate Various resin films such as ethylene glycol ester (PEN), polycarbonate (PC), polyimide (PI), ethylene-tetrafluoroethylene copolymer (ETFE), and heat-resistant transparent films and laminates with organic-inorganic hybrid structure One of the resin films composed of two or more resin layers; it can also be a substrate deposited with a functional layer, including a substrate coated with a solar cell functional layer, a light-emitting diode functional layer, and an electrochromic functional layer.
[0065] The specific preparation steps of the ultra-thin silver-based film are as follows:
[0066] (1) Put the substrate 1 on the substrate stage in the cavity of the magnetron sputtering thin film deposition equipment pre-installed with high-purity Ag targets;
[0067] (2) Pump the background vacuum of the cavity of the magnetron sputtering equipment to 1.0×10 -3 Below Pa, pass argon gas and an appropriate amount of oxygen into the cavity, sputter a high-purity Ag target in an argon-oxygen mixed gas atmosphere, and deposit an Ag(O) layer 2 on the substrate 1;
[0068] (3) Without destroying the vacuum of the deposition chamber, pump the vacuum of the chamber to 1.0×10 -3 After Pa is below Pa, argon is introduced into the cavity, a high-purity Ag target is sputtered in an argon atmosphere, and an Ag layer 3 is deposited on the Ag(O) layer 2.

Example Embodiment

[0069] Example 2
[0070] Such as figure 2 As shown, a multilayer composite transparent conductive film includes a substrate 1 and at least two layers of Ag(O)/Ag double-layer stacking structure. Specifically, a first Ag(O) layer 2 and a second Ag(O) layer are sequentially arranged on the substrate 1. An Ag layer 3, a second Ag(O) layer 21 and a second Ag layer 31.
[0071] The preparation method of the multilayer composite transparent conductive film is as follows:
[0072] (1) Put the substrate 1 on the substrate stage in the cavity of the magnetron sputtering thin film deposition equipment pre-installed with high-purity Ag targets;
[0073] (2) Pump the background vacuum of the cavity of the magnetron sputtering equipment to 1.0×10 -3 Below Pa, pass argon gas and an appropriate amount of oxygen into the cavity, sputter a high-purity Ag target under an argon-oxygen mixed gas atmosphere, and deposit a first Ag(O) layer 2 on the substrate 1;
[0074] (3) Without destroying the vacuum of the deposition chamber, pump the vacuum of the chamber to 1.0×10 -3 After Pa is below Pa, argon is introduced into the cavity, a high-purity Ag target is sputtered in an argon atmosphere, and the first Ag layer 3 is deposited on the Ag(O) layer;
[0075] (4) Without destroying the vacuum of the deposition chamber, pump the vacuum of the chamber to 1.0×10 -3 After Pa is below Pa, argon gas and an appropriate amount of oxygen are passed into the cavity, a high-purity Ag target is sputtered in an argon-oxygen mixed gas atmosphere, and a second Ag(O) layer 21 is deposited on the first Ag layer 3;
[0076] (5) Without destroying the vacuum of the deposition chamber, pump the vacuum of the chamber to 1.0×10 -3 After Pa is below Pa, argon is introduced into the cavity, a high-purity Ag target is sputtered in an argon atmosphere, and a second Ag layer 31 is deposited on the second Ag(O) layer 21.

Example Embodiment

[0077] Example 3
[0078] Such as image 3 As shown, a multilayer composite transparent conductive film includes a substrate 1, an Ag(O) layer 2, an Ag layer 3, a bottom layer 4, and a top layer 5. The bottom layer 4 is arranged between the substrate 1 and the Ag(O) layer 2, It is used to enhance adhesion, work function matching, protection, anti-reflection or any combination of these properties; the top layer 5 is disposed above the Ag layer 3, which is used for anti-reflection, work function matching, protection or any combination of these properties.
[0079] The substrate 1 can be a dielectric, semiconductor or metal substrate, including glass, quartz, silicon wafer, stainless steel, etc.; it can also be an organic polymer substrate, including polyethylene terephthalate (PET), polyethylene naphthalate Various resin films such as ethylene glycol ester (PEN), polycarbonate (PC), polyimide (PI), ethylene-tetrafluoroethylene copolymer (ETFE), and heat-resistant transparent films and laminates with organic-inorganic hybrid structure One of the resin films composed of two or more resin layers; it can also be a substrate deposited with a functional layer, including a substrate coated with a solar cell functional layer, a light-emitting diode functional layer, and an electrochromic functional layer.
[0080] The material of the top or bottom layer can be a semiconductor material or a dielectric material, such as indium tin oxide (ITO), aluminum-doped zinc oxide (AZO), fluorine-doped tin oxide (FTO), gallium-doped zinc oxide (GZO), tin oxide ( SnO 2 ), zinc oxide (ZnO), titanium oxide (TiO 2 ), tungsten oxide (WO 3 ), molybdenum oxide (MoO 3 ), nickel oxide (NiO), copper oxide (CuO) and other binary or multi-component transparent oxides, or other compound semiconductors such as ZnS, CdS, PbSe, CdSe, CdTe, CuS, etc.
[0081] The preparation method of the multilayer composite transparent conductive film is as follows:
[0082] Step 1: Use PET film as the substrate, ultrasonically clean the PET substrate with acetone, ethanol, and deionized water, and then use dry N 2 Blow dry and bake in the oven to 60°C for 10 minutes. Then put the PET substrate into the cavity of a multi-target radio frequency magnetron sputtering thin film deposition equipment, which is pre-installed with AZO targets (made of ZnO and Al). 2 O 3 Composition, where Al 2 O 3 (Accounting for 3% of the total mass of the AZO target), 99.99% purity Ag target, each layer of the silver-based multilayer composite transparent conductive film is prepared by RF magnetron sputtering technology, and the RF power frequency for sputtering is 13.56 MHz .
[0083] Step 2: Use mechanical pumps and molecular pumps to pump the vacuum of the magnetron sputtering equipment to 1.0×10 -4 Pa, then 30 sccm of argon gas was introduced, the pressure was adjusted to 0.5 Pa, the sputtering power was 150 W, and the 45 nm bottom AZO layer was deposited on the substrate by controlling the coating time.
[0084] Step 3: After the bottom layer AZO is deposited, without breaking the vacuum of the deposition chamber, continue to deposit the Ag(O) transition layer in the chamber. The specific steps are: pre-sputtering the silver target first to remove the oxide layer that may exist on the surface of the silver target to ensure the repeatability of each process. The pre-sputtering conditions are 30 sccm of argon gas, 0.7 Pa pressure, 30 W sputtering power, and 5 minutes sputtering time. After the pre-sputtering of the silver target is completed, the deposition of the Ag(O) transition layer is started. Turn off the argon gas introduced during the pre-sputtering, and use the mechanical pump and molecular pump to pump the vacuum of the magnetron sputtering equipment to 1.0×10 -4 After Pa, a mixture of 30 sccm of argon and oxygen (volume ratio of oxygen is 1%) is introduced, the pressure is adjusted to 0.6 Pa, and the sputtering power is 40 W. The deposited Ag(O) can be achieved by adjusting the deposition time. The layer thickness is controlled, and the oxygen doping concentration x in the Ag(O) layer is 8.4%.
[0085] Step 4: Turn off the argon-oxygen mixture in step 3, without destroying the vacuum of the deposition chamber, continue to deposit the Ag film in the chamber, and use the mechanical pump and molecular pump to pump the vacuum of the magnetron sputtering equipment to 1.0 ×10 -4 Pa, then 30sccm of argon gas was introduced, the pressure was adjusted to 0.7 Pa, and the sputtering power was 30 W. The thickness of the deposited Ag layer can be controlled by adjusting the deposition time.
[0086] Step 5: Without destroying the vacuum of the deposition chamber, repeat step 2, and then deposit a 45 nm AZO layer on it to obtain the AZO(45nm)/Ag(O)/Ag/AZO(45nm) multilayer composite of Example 2 Transparent conductive film.
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PUM

PropertyMeasurementUnit
Thickness0.5 ~ 5.0nm
Thickness2.0nm
Total thickness8.0nm
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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