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CN-122013119-A - Physical vapor deposition equipment, electrochromic device and preparation method thereof

CN122013119ACN 122013119 ACN122013119 ACN 122013119ACN-122013119-A

Abstract

The application discloses physical vapor deposition equipment, an electrochromic device and a preparation method thereof, and relates to the technical field of electrochromic devices. The preparation method comprises the steps of performing sputter deposition on a WO 3 electrochromic layer on the surface of a first ITO layer, wherein the oxygen content is any one value of 42.5% -52.5%, performing sputter deposition on a tungsten oxide ion conducting layer with a preset thickness on the electrochromic layer, wherein the oxygen content of a corresponding chamber is any one value of 35% -45%, performing sputter deposition on an ion storage layer containing lithium ions on the ion conducting layer, performing vacuum annealing treatment and cooling treatment on a second ITO layer, and preparing the electrochromic device, wherein the deposition temperature of the second ITO layer is any one value of 350-400 ℃, and the annealing temperature of the vacuum annealing treatment is any one value of 450-500 ℃. The electrochromic device prepared by the application has higher transmittance and low sheet resistance.

Inventors

  • HE GANG
  • ZHANG JING
  • HAN ZHONGPENG
  • Chen Yeyue

Assignees

  • 苏州伯宇光电科技有限公司

Dates

Publication Date
20260512
Application Date
20260416

Claims (10)

  1. 1. The preparation method of the electrochromic device based on the physical vapor deposition process is characterized by comprising the following steps of: Sputtering and depositing an electrochromic layer on the surface of the first ITO layer above the substrate, wherein the material of the electrochromic layer is WO 3 , and the oxygen content of a corresponding chamber is any value of 42.5% -52.5%; sputtering and depositing an ion conducting layer with a preset thickness of any value of 200-500 nm on the electrochromic layer, wherein the ion conducting layer is a non-stoichiometric tungsten oxide layer with an oxygen vacancy structure, and the oxygen content of a corresponding chamber is any value of 35-45%; Sequentially sputtering and depositing an ion storage layer and a lithium ion-containing layer on the ion conducting layer, wherein the ion storage layer is a nickel oxide layer with an amorphous structure, so that lithium ions in the lithium ion-containing layer are diffused and stored in the ion storage layer, the deposition temperature of the ion storage layer is any value from 350 ℃ to 400 ℃, and the oxygen content of a corresponding chamber is any value from 80% to 87%; Depositing a second ITO layer on the ion storage layer, and sequentially carrying out vacuum annealing treatment and cooling treatment to prepare the electrochromic device, The deposition temperature of the second ITO layer is any value of 350-400 ℃, the annealing temperature of the vacuum annealing treatment is any value of 450-500 ℃, the annealing time is any value of 480-900 s, and the vacuum degree is less than 6.0X10 -4 Pa.
  2. 2. The method for fabricating an electrochromic device based on a physical vapor deposition process according to claim 1, wherein, When the vacuum annealing treatment is carried out, a first constant temperature chamber and a second constant temperature chamber are respectively arranged between the chamber where the vacuum annealing treatment is arranged and the chamber where the second ITO layer is deposited and between the chamber where the vacuum annealing treatment is arranged and the chamber where the cooling treatment is arranged, and the temperatures of the first constant temperature chamber and the second constant temperature chamber are all 380 ℃ to 400 ℃.
  3. 3. The method for fabricating an electrochromic device based on a physical vapor deposition process according to claim 1, wherein, Before depositing the lithium ion-containing layer, the substrate is passed through a first isolation chamber disposed between the chamber in which the ion storage layer is deposited and the chamber in which the lithium ion-containing layer is deposited to temperature transition the substrate and block gas flow.
  4. 4. The method for fabricating an electrochromic device based on a physical vapor deposition process according to claim 1, wherein, After depositing the lithium ion-containing layer, the substrate is passed through a second isolation chamber disposed between the chamber in which the lithium ion-containing layer is deposited and the chamber in which the second ITO layer is deposited to temperature transition the substrate and block gas flow.
  5. 5. The method for fabricating an electrochromic device based on a physical vapor deposition process according to claim 1, wherein, Before depositing the lithium ion-containing layer, pumping treatment is carried out in an isolation chamber between the chamber for depositing the ion storage layer and the chamber for depositing the lithium ion-containing layer, so as to reduce the water vapor content carried by the substrate before entering the chamber for depositing the lithium ion-containing layer.
  6. 6. The method of fabricating an electrochromic device based on a physical vapor deposition process according to any one of claims 1-5, further comprising, prior to the step of sputter depositing an electrochromic layer on the surface of the first ITO layer located over the substrate: And sequentially performing cleaning treatment and preheating treatment on the first ITO layer arranged on the substrate.
  7. 7. The method of manufacturing an electrochromic device based on a physical vapor deposition process according to claim 6, wherein, The deposition temperature of the electrochromic layer is any value from 200 ℃ to 300 ℃.
  8. 8. The method for manufacturing an electrochromic device based on a physical vapor deposition process according to claim 7, wherein, The deposition temperature of the ion conducting layer is any one of 200 ℃ to 300 ℃; the deposition temperature of the lithium ion-containing layer is any value from 90 ℃ to 110 ℃.
  9. 9. A physical vapor deposition apparatus for carrying out the physical vapor deposition-based electrochromic device manufacturing method according to any one of claims 1 to 8, characterized by comprising a first tungsten deposition chamber, a second tungsten deposition chamber, a nickel deposition chamber, a lithium deposition chamber, an ITO deposition chamber, a vacuum annealing chamber, and a cooling chamber, which are sequentially arranged in a production process direction.
  10. 10. An electrochromic device prepared and obtained by the physical vapor deposition process-based electrochromic device preparation method according to any one of claims 1-8, characterized by comprising a substrate, a first ITO layer, an electrochromic layer, an ion conducting layer, an ion storage layer and a second ITO layer, which are sequentially stacked from bottom to top, wherein the thickness of the ion conducting layer is any one of 200nm-500nm, and the ion storage layer is a nickel oxide layer with lithium ions distributed.

Description

Physical vapor deposition equipment, electrochromic device and preparation method thereof Technical Field The invention relates to the technical field of electrochromic devices, in particular to physical vapor deposition equipment, an electrochromic device and a preparation method thereof. Background The electrochromic device can realize color change under the action of an applied voltage, and is widely applied to the fields of electrochromic lenses, intelligent windows and displays. In practical application, the device is required to have not only good electrochromic response performance, but also higher light transmittance and lower haze, so that the optical performance requirement is met. Currently, electrochromic devices generally employ physical vapor deposition processes to produce multi-layer functional structures, including electrochromic layers, ion conducting layers, ion storage layers, and the like. The electrochromic performance of the tungsten oxide is dependent on the intercalation and deintercalation process of lithium ions, and meanwhile, the ion conducting layer and the ion storage layer have important influence on the transmission efficiency and the storage capacity of lithium ions. However, in the prior art, the above functional layers often lack accurate control over oxygen content during the deposition process, which easily causes deviation of the electrochromic layer from an ideal stoichiometric ratio, insufficient or excessive defect structure of the ion conducting layer, and unstable structure of the ion storage layer, thereby affecting migration efficiency and storage stability of lithium ions, and further reducing response speed and cycle performance of the electrochromic device. In addition, during the preparation and post-treatment of the electrode layer, the prior art generally employs low temperature conditions to deposit the ITO layer and subsequently performs an annealing treatment to improve its conductive properties. However, the ITO film formed by low-temperature deposition is easy to generate structural change under the high-temperature vacuum annealing condition, so that the sheet resistance is obviously increased, and in order to avoid the problem, part of technical schemes adopt atmospheric environment annealing, but the mode has the problems of long annealing time and easy introduction of oxygen and water vapor, thereby influencing the activity of lithium ions, and causing the optical performance of electrochromic devices to be reduced and the consistency of products to be poor. Therefore, the prior art is difficult to realize the cooperative optimization of the electrochromic layer performance, the ion transmission performance and the electrode conductivity in the multi-layer structure deposition process, and especially has the defects in the aspects of oxygen content regulation and ITO deposition and vacuum annealing process matching, so that an improved electrochromic device preparation method is needed to improve the overall performance and stability of the device. Disclosure of Invention An object of the first aspect of the present invention is to provide a method for preparing an electrochromic device based on a physical vapor deposition process, which solves the technical problems that in the prior art, in the preparation process of the electrochromic device, the oxygen content of each functional layer is not regulated enough, so that the ion transmission and storage performance are unstable, the resistance of a low-temperature deposited ITO layer is increased under the vacuum high-temperature annealing condition, and the atmospheric annealing is easy to influence the lithium ion activity. Another object of the first aspect of the present invention is to maintain the high crystallinity and low sheet resistance characteristics of the second ITO layer. It is an object of a second aspect of the present invention to provide a physical vapor deposition apparatus for carrying out the above-described preparation method. An object of a third aspect of the present invention is to provide an electrochromic device prepared according to the above-described preparation method. According to an object of a first aspect of the present invention, the present invention provides a method for manufacturing an electrochromic device based on a physical vapor deposition process, comprising the steps of: Sputtering and depositing an electrochromic layer on the surface of the first ITO layer above the substrate, wherein the material of the electrochromic layer is WO 3, and the oxygen content of a corresponding chamber is any value of 42.5% -52.5%; sputtering and depositing an ion conducting layer with a preset thickness of any value of 200-500 nm on the electrochromic layer, wherein the ion conducting layer is a non-stoichiometric tungsten oxide layer with an oxygen vacancy structure, and the oxygen content of a corresponding chamber is any value of 35-45%; Sequentially sputtering and