CN110904418A

CN110904418A - Preparation method of low-radiation composite film

Info

Publication number: CN110904418A
Application number: CN201911258559.3A
Authority: CN
Inventors: 黄丽莎; 姜菊美
Original assignee: JIANGSU AOLAN ARCHITECTURE GLASS CO Ltd
Current assignee: JIANGSU AOLAN ARCHITECTURE GLASS CO Ltd
Priority date: 2019-12-10
Filing date: 2019-12-10
Publication date: 2020-03-24

Abstract

The invention discloses a preparation method of a low-radiation composite film, which comprises the following steps of S1: preparation of a first layer of Ti0 by RF reactive magnetron sputtering₂Ti is adopted as a target material, and 0 is introduced during sputtering₂Reacting to form Ti0₂Deposited on a substrate, forming a layer of TiO on the target surface during sputtering₂Applying a radio frequency voltage to the Ti target, S2: preparing Ag layer by DC magnetron sputtering method, rotating the substrate, and reducing sputtering current to0.2A, power 150W, sputtering power was reduced, and the substrate was selected for a round time of 2 minutes to pass the substrate 5 times on top of the Ag layer, S3: preparing a composite film, and preparing a third Ti0 layer on the Ag layer₂Preparing a third layer of Ti0₂In the same manner as in S1, in preparing a third Ti0 layer₂When in use, a Ti layer is additionally plated on the Ag layer, and the Ag layer is protected by the Ti layer. The invention can protect the Ag layer and reduce the thickness of the film, thereby improving the light transmittance and improving the service performance.

Description

Preparation method of low-radiation composite film

Technical Field

The invention relates to the technical field of composite films, in particular to a preparation method of a low-radiation composite film.

Background

The low-radiation film is developed in the development process of large-area glass coating, and hollow glass and vacuum glass have a certain energy-saving and heat-insulating effect due to the fact that the hollow glass and the vacuum glass effectively prevent convection and conduction of heat and have a certain energy-saving and heat-insulating effect, and have widely entered daily production and life of people. But the energy-saving effect of the common hollow glass is only 60% 2, and the heat-insulating effect is not obvious. The low-radiation glass (low-e glass) has larger visible light transmittance and smaller infrared reflection coefficient, can allow more than 80% of visible light to enter the room, and reflects more than 90% of sunlight and infrared rays radiated by indoor objects, has more than 75% of energy-saving effect, and can meet the requirements of lighting, decoration, light pollution prevention and the like of buildings. The low-radiation glass is the most ideal energy-saving material for windows due to excellent energy-saving and environment-friendly performance, and the low-radiation film glass is widely applied to building energy-saving window glass due to the advantages of reflecting infrared rays and ultraviolet rays, having better transmittance for visible light and the like.

The preparation methods of the low-radiation film are divided into two major categories, namely an online method and an offline method. According to different methods, the low-radiation film is also divided into two types of different structures, namely an online film and an offline film, the online method adopts a high-temperature pyrolysis method of chemical tear deposition to produce the low-radiation film, the offline method is a method for plating the low-radiation film on the surface of glass by magnetron sputtering and other methods after the glass is offline, the film plated by the method is called the offline film, also called a soft film, the structure of the offline film is generally a sandwich structure of a dielectric layer/a metal layer/a dielectric layer (DMD), a metal shell adopts gold, silver, aluminum and the like, the thickness is generally within 20nm, and the metal film can form a continuous film and is transparent under the thickness. Thus, most of visible light can be allowed to pass through, but most of infrared light and ultraviolet light can be reflected off, and since the metal film is not wear-resistant, dielectric films need to be plated on two sides of the metal film. Generally, a metal oxide film (TiOx, SnOx, Znox, etc.) or a similar insulating film, and an inner dielectric film are used to improve the adhesion between silver and the glass surface and to adjust the optical properties and color of the film system. The outer dielectric film is both an antireflective film and a protective film. It can improve the solar transmittance in this wavelength range while protecting the metal film. Both sides are less than one quarter of the optical wavelength thick. Also, the higher the refractive index of the dielectric thin film, the higher the transmittance of the entire film.

In the process of implementing the invention, the inventor finds that at least the following problems in the prior art are not solved: 1. the whole thickness of the film is higher, so that the light transmittance of the film is influenced, and the service performance of the film is reduced; 2. in the process of preparing the Ag layer, oxidation easily occurs, so that the oxidation and TiO are influenced₂The binding rate of (4).

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides the preparation method of the low-radiation composite film, which can protect the Ag layer and reduce the thickness of the film, thereby improving the light transmittance and the service performance of the film.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme:

a preparation method of a low-radiation composite film comprises the following steps:

s1: preparation of the first layer Ti0₂Firstly, pumping the air pressure in a vacuum chamber to a certain degree, preheating a radio frequency power supply for a certain time, then introducing working gas argon, adopting Ti as a target material, and introducing 0 during sputtering₂Reacting to form Ti0₂Deposited on a substrate, forming a layer of TiO on the target surface during sputtering₂Applying radio frequency voltage to the Ti target;

s2: preparing Ag layer by closing argon as reaction working gas and vacuumizing to 5x10^- ³Pa, simultaneously turning on a silver target radio frequency power supply to preheat for 10 minutes, introducing argon into the vacuum chamber to adjust the radio frequency power of the silver target to glow when the two reach specified values, rotating the substrate in the preparation process, reducing the sputtering current to 0.2A and the power to 150W, and reducing the sputtering powerSelecting a circle of time as 2 minutes for the substrate to pass 5 times on the upper part of the Ag layer;

s3: preparing a composite film, and preparing a third Ti0 layer on the Ag layer₂The working argon is turned off, and vacuum is re-pumped by 5x10^- ³Pa, preparing a third layer of Ti0₂In the same manner as in S1, in preparing a third Ti0 layer₂And then, plating a Ti layer on the Ag layer, adjusting the power to 200% by adopting radio frequency sputtering, and protecting the Ag layer by the Ti layer, wherein the sputtering time is 20 s.

Preferably, Ti0 in S1₂The preparation method is carried out by adopting a radio frequency reaction magnetron sputtering method.

Preferably, the starting pressure of the sputtering in S1 is 2Pa, and the power is 300 w.

Preferably, the vacuum chamber pressure in S1 is 5x10^-3Pa。

Preferably, the preheating time of the rf power supply in S1 is ten minutes.

Preferably, in the sputtering process in S1, the pressure is reduced to 1Pa, the partial pressure ratio of oxygen to argon is 1:2, the sputtering time is 10 minutes, and the temperature is normal temperature.

Preferably, the Ag layer in S2 is prepared by a dc magnetron sputtering method.

Preferably, the Ti layer has a thickness of 1nm and is judged by time characterization.

(III) advantageous effects

The invention provides a preparation method of a low-radiation composite film, which has the following beneficial effects:

the substrate is rotated in the process of preparing the Ag layer, so that the sputtering area can be reduced, the thickness of the Ag layer is reduced, the overall thickness of the film is reduced, the Ti-plated layer is additionally plated on the Ag layer to protect the Ag layer, and the situation that 0 is introduced can be prevented₂The Ag layer is oxidized, and the light transmittance of the film is improved.

Drawings

FIG. 1 is a flow chart of a preparation method of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The first embodiment is as follows: referring to fig. 1, the preparation method of the low-emissivity composite film provided by the invention comprises the following steps:

s1: preparation of the first layer Ti0₂Firstly, the air pressure in the vacuum chamber is pumped to 5x10^-3Pa, preheating for ten minutes by using a radio frequency power supply, then introducing working gas argon, and preparing Ti0 by adopting a radio frequency reaction magnetron sputtering method₂Ti is adopted as a target material, and 0 is introduced during sputtering₂Reacting to form Ti0₂Deposited on a substrate, to form a thin layer of TiO on the target surface during sputtering₂Applying radio frequency voltage on Ti target, preparing Ti0 by radio frequency reaction magnetron sputtering₂The starting pressure of sputtering is 2Pa, the power is 300w, the pressure is reduced to 1Pa in the sputtering process, the partial pressure ratio of oxygen to argon is 1:2, the height of the substrate from the target surface is 11.7cm, the sputtering time is 10 minutes, and the temperature is normal temperature;

s2: preparing an Ag layer by adopting a direct current magnetron sputtering method, closing a reaction working gas argon before preparation, and vacuumizing a vacuum chamber to 5x10^-3Pa, simultaneously turning on a silver target radio-frequency power supply to preheat for 10 minutes, introducing argon into the vacuum chamber to adjust the radio-frequency power of the silver target to glow when the two reach specified values, rotating the substrate in the preparation process, reducing the sputtering current to 0.2A and the power to 150W, reducing the sputtering power, and enabling the substrate to pass through the upper part of the Ag layer for 5 times by selecting a circle of time for 2 minutes;

s3: preparing a composite film, and preparing a third Ti0 layer on the Ag layer₂The working argon is turned off, and vacuum is re-pumped by 5x10^- ³Pa, preparing a third layer of Ti0₂In the same manner as in S1, in preparing a third Ti0 layer₂In which a Ti layer is additionally plated on the Ag layerThe thickness is 1nm, the thickness of the Ti layer is judged through time characterization, radio frequency sputtering is adopted, the power is adjusted to be 200%, the sputtering time is 20s, and the Ag layer is protected through the Ti layer, so that the composite film is obtained.

According to the invention, in the process of preparing the Ag layer, the substrate is rotated, so that the sputtering area can be reduced, the thickness of the Ag layer is reduced, the overall thickness of the film is reduced, the Ti-plated layer is additionally arranged on the Ag layer for protecting the Ag layer, and O can be prevented from being introduced₂When the Ag layer is oxidized, the light transmittance of the film is improved.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation. The element defined by the sentence "comprising one.. said, does not exclude the presence of additional identical elements in the process, method, article or apparatus comprising said element, the electrical elements presented therein are all electrically connected to an external master and 220V mains, and the master may be a conventionally known apparatus, such as a computer, which acts as a control.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The preparation method of the low-radiation composite film is characterized by comprising the following steps of:

s1: system for makingPreparing the first layer of TiO₂Firstly, pumping the air pressure in a vacuum chamber to a certain degree, preheating a radio frequency power supply for a certain time, then introducing working gas argon, adopting Ti as a target material, and introducing O during sputtering₂To react to form TiO₂Deposited on a substrate, forming a layer of TiO on the target surface during sputtering₂Applying radio frequency voltage to the Ti target;

s2: preparing Ag layer by closing argon as reaction working gas and vacuumizing to 5x10^-3Pa, simultaneously turning on a silver target radio-frequency power supply to preheat for 10 minutes, introducing argon into the vacuum chamber to adjust the radio-frequency power of the silver target to glow when the two reach specified values, rotating the substrate in the preparation process, reducing the sputtering current to 0.2A and the power to 150W, reducing the sputtering power, and enabling the substrate to pass through the upper part of the Ag layer for 5 times by selecting a circle of time for 2 minutes;

s3: preparing a composite film, and preparing a third Ti0 layer on the Ag layer₂The working argon is turned off, and vacuum is re-pumped by 5x10^-3Pa, preparation of the third layer of TiO₂In the same manner as in S1, in the preparation of the third layer of TiO₂And then, plating a Ti layer on the Ag layer, adjusting the power to 200% by adopting radio frequency sputtering, and protecting the Ag layer by the Ti layer, wherein the sputtering time is 20 s.

2. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: TiO in the S1₂The preparation method is carried out by adopting a radio frequency reaction magnetron sputtering method.

3. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: the starting pressure of the sputtering in the S1 is 2Pa, and the power is 300 w.

4. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: the vacuum chamber pressure in S1 is 5x10^-3Pa。

5. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: the preheating time of the radio frequency power supply in the S1 is ten minutes.

6. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: in the sputtering process of S1, the pressure is reduced to 1Pa, the partial pressure ratio of oxygen to argon is 1:2, the sputtering time is 10 minutes, and the temperature is normal temperature.

7. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: the Ag layer in the S2 is prepared by a direct-current magnetron sputtering method.

8. The method for preparing a low-emissivity composite film according to claim 1, wherein the method comprises: the thickness of the Ti layer was 1nm and was judged by time characterization.