HK1215564A1 - Coated glass and preparation method thereof - Google Patents
Coated glass and preparation method thereof Download PDFInfo
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- HK1215564A1 HK1215564A1 HK16103574.0A HK16103574A HK1215564A1 HK 1215564 A1 HK1215564 A1 HK 1215564A1 HK 16103574 A HK16103574 A HK 16103574A HK 1215564 A1 HK1215564 A1 HK 1215564A1
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Description
Technical Field
The invention relates to the technical field of coated glass, in particular to coated glass adopting a novel barrier technology and having thermal stability and a preparation method thereof.
Background
The silver-based Low-Emissivity (Low-E) coated glass is prepared by depositing a plurality of layers of metal films and dielectric films on the surface of float glass, and a coated product with good optical property, electrical property and thermal property can be obtained by properly selecting materials and optimizing the film system structure. Low-E coated glass is one of the most widely used materials in building energy-saving products due to the excellent far infrared reflection characteristic. The three-silver Low-emissivity coated glass is a Low-E product with the highest technical content in the field at present, and a film system of the three-silver Low-emissivity coated glass comprises more than ten film layers such as a dielectric layer, a barrier layer, a metal layer and the like.
However, the existing three-silver low-emissivity coated glass has the problems that the transmittance is low and products before and after toughening cannot be mixed. The reason is that the existing Low-E film system mostly adopts metal materials as barrier layers, such as NiCr, Ti, Cr and the like, so as to protect the silver layer from being affected by the subsequent sputtering process and prevent the silver layer from being damaged in the toughening process. However, the metal film absorbs light, so that the transmittance of the three-silver Low-E coated glass is difficult to improve. In addition, in the toughening process, the metal material is used as a sacrificial layer to absorb oxygen and partially or completely change into metal oxide, the transmittance of the Low-E product is obviously increased after toughening, and the color is greatly changed, so that the coated glass products obtained before and after toughening cannot be mixed.
The utility model with the publication number of CN202448400U adopts a composite barrier layer structure, namely a metal barrier layer/AZO barrier layer, to improve the visible light transmittance of the low-radiation coated glass with a temperable double-function layer structure and reduce the color change after tempering. Although effective, the two barrier layers mean that the production line needs to be equipped with one more sputtering chamber, which adds additional capital investment to the equipment. In addition, in CN202448400U patent, the intermediate frequency power source and the rotating cathode are used to sputter deposit AZO, and this production method has a problem: after the AZO target is installed and used for a period of time, the surface of the AZO target is easy to generate a nodulation discharge phenomenon and even generates slag, the service power and the service life of the target are seriously influenced, a production line is sometimes forced to return air in advance, residues are cleaned, and the production efficiency is reduced.
Disclosure of Invention
The invention provides coated glass with thermal stability by adopting a novel barrier technology and a preparation method thereof.
According to a first aspect of the present invention, the present invention provides a coated glass, comprising a glass substrate and a film layer formed on the glass substrate, wherein the film layer comprises, in order from the glass substrate to the outside: the infrared reflection coating comprises a first composite dielectric layer, a first infrared reflection layer, a first barrier layer, a second composite dielectric layer, a second infrared reflection layer, a second barrier layer, a third composite dielectric layer, a third infrared reflection layer, a third barrier layer and a fourth composite dielectric layer, wherein the first barrier layer, the second barrier layer and the third barrier layer are prepared by sputtering a metal oxide ceramic target by a direct-current power supply, and the metal oxide ceramic target is selected from AZO and TiOxOr NiCrOxAnd is a rotating target.
In a preferred embodiment of the present invention, the first barrier layer, the second barrier layer, and the third barrier layer each have a thickness of 0.5 to 5 nm.
In a preferred embodiment of the present invention, the first infrared reflecting layer, the second infrared reflecting layer, and the third infrared reflecting layer are made of silver or a silver alloy.
In a preferred embodiment of the present invention, the first infrared reflecting layer, the second infrared reflecting layer, and the third infrared reflecting layer are made of a silver alloy, the silver alloy mainly contains silver and at least one element selected from gold, titanium, palladium, copper, and niobium, and the content of the at least one element selected from gold, titanium, palladium, copper, and niobium is 0.3 to 10at.% based on the total amount of the silver alloy.
In a preferred embodiment of the present invention, the first infrared reflective layer, the second infrared reflective layer, and the third infrared reflective layer each have a thickness of 5 to 15 nm.
As a preferred embodiment of the present invention, the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are Si3N4、SnO2、Zn2SnO4、Nb2O5And ZnAlOxTwo or more of them are combined into a film layer.
As a preferred scheme of the invention, the thicknesses of the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are respectively 10-85 nm.
As a preferable scheme of the invention, the coated glass further comprises a protective layer outside the fourth composite dielectric layer, and the protective layer is TiO2、Si3N4、SiNxOyOr ZrO2At least one of (1) and (2) has a thickness of 5 to 30 nm.
According to a second aspect of the present invention, there is provided a method of producing the coated glass of the first aspect, the method comprising: forming film layers in the following sequence from the glass substrate to the outside on the glass substrate through sputtering: the method comprises the steps of preparing a first barrier layer, a second barrier layer and a third barrier layer by sputtering a metal oxide ceramic target by using a direct current power supply, wherein the metal oxide ceramic target is selected from AZO and TiOxOr NiCrOxAnd is a rotating target.
As a preferred scheme of the invention, if the AZO is selected as the target material of the barrier layer, pure argon is used as the sputtering gas, and no reaction gas is added; if TiO is selectedxOr NiCrOxAs the target material of the barrier layer, a mixed gas of argon and oxygen is used as the sputtering gas, wherein the volume of the oxygen containsThe amount is 10% or less, preferably 7% or less.
In a preferred embodiment of the present invention, the first barrier layer, the second barrier layer, and the third barrier layer each have a thickness of 0.5 to 5 nm.
As a preferable scheme of the invention, the method adopts a direct current power supply and a planar cathode to form the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer by sputtering deposition in an argon atmosphere.
In a preferred embodiment of the present invention, the first infrared reflective layer, the second infrared reflective layer, and the third infrared reflective layer each have a thickness of 5 to 15 nm.
In a preferred embodiment of the present invention, the first infrared reflecting layer, the second infrared reflecting layer, and the third infrared reflecting layer are made of silver or a silver alloy.
In a preferred embodiment of the present invention, the first infrared reflecting layer, the second infrared reflecting layer, and the third infrared reflecting layer are made of a silver alloy, the silver alloy mainly contains silver and at least one element selected from gold, titanium, palladium, copper, and niobium, and the content of the at least one element selected from gold, titanium, palladium, copper, and niobium is 0.3 to 10at.% based on the total amount of the silver alloy.
According to the preferred scheme of the invention, the method adopts intermediate-frequency alternating-current voltage and a double-rotating cathode to form the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer by sputtering and deposition in an argon-nitrogen or argon-oxygen mixed atmosphere.
As a preferred scheme of the invention, the thicknesses of the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are respectively 10-85 nm.
As a preferred embodiment of the present invention, the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are Si3N4、SnO2、Zn2SnO4、Nb2O5And ZnAlOxTwo or more of them are combined into a film layer.
As a preferable embodiment of the present invention, the method further includes forming a protective layer by sputtering outside the fourth composite dielectric layer, where the protective layer is TiO2、Si3N4、SiNxOyOr ZrO2At least one of (1) and (2) has a thickness of 5 to 30 nm.
In a preferred embodiment of the present invention, the protective layer is formed by sputter deposition using a medium-frequency ac voltage and a dual-rotating cathode in a mixed atmosphere of argon nitrogen or argon oxygen.
Each barrier layer of the coated glass has only one layer and is prepared by sputtering a metal oxide ceramic target (rotating target) by a direct current power supply, wherein the metal oxide ceramic target is selected from AZO and TiOxOr NiCrOxOne kind of (1). The novel barrier technology avoids the problem that the absorption characteristic of the barrier layer is changed before and after tempering, and is beneficial to preparing the low-emissivity coated glass with thermal stability. Meanwhile, the novel blocking technology adopts a direct-current power supply to sputter the rotating target, avoids the problems of arc striking or slag falling and the like of the ceramic target, and solves the technical problem of the AZO target in the actual production. In addition, the metal oxide barrier layer prepared by the process has the dual characteristics of metal and dielectric, and the barrier layer has low absorption to visible light, so that the metal oxide barrier layer can be used as a protective layer of a silver layer or a silver alloy layer and can also be used as a dielectric layer. Particularly, in the toughening process, the metal oxide barrier layer has a positive effect on the stability of the film structure and the color stability. Because the metal oxide barrier layer can not generate obvious optical property change when being heated, the metal oxide barrier layer can play a role in blocking oxygen and can effectively protect the silver layer from being damaged.
Therefore, the coated glass has the advantages that: (1) the product has high transmittance, and the visible light transmittance is more than or equal to 60 percent; (2) the color stability of the product before and after tempering is good; (3) the product has excellent moisture resistance.
Drawings
FIG. 1 is a schematic structural view of a coated glass according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
Referring to fig. 1, the coated glass of the present invention includes a glass substrate and a film layer formed on the glass substrate, the film layer sequentially includes, from the glass substrate to the outside: the infrared reflection layer comprises a first composite dielectric layer, a first infrared reflection layer, a first barrier layer, a second composite dielectric layer, a second infrared reflection layer, a second barrier layer, a third composite dielectric layer, a third infrared reflection layer, a third barrier layer, a fourth composite dielectric layer and an optional protective layer.
It should be noted that fig. 1 is only a schematic structural diagram of the coated glass, wherein each film layer is only schematic, and the actual thickness of the film layer is not as shown in fig. 1.
The key point of the present invention is that the first barrier layer, the second barrier layer and the third barrier layer are prepared by sputtering a metal oxide ceramic target using a direct current power source, which is a technical means never adopted in the prior art. The metal oxide ceramic target in the invention is selected from AZO and TiOxOr NiCrOxAnd is a rotating target.
Wherein AZO is aluminum-doped zinc oxide, and the AZO adopted in one embodiment of the invention has the composition of 98 wt% ZnO and 2 wt% Al2O3；TiOxIs an oxide of titanium, as a sputtering target, which has the known characteristics in the field of sputtering targets, generally is an oxide in a non-complete oxidation state, wherein the value range of x can be within the range of 1.6-1.9; NiCrOxIs a nickel chromium oxide having the characteristics known in the art of sputtering targets, typically an oxide in a non-fully oxidized state, wherein x can range from 0.5 to less than or equal tox is less than or equal to 1.
In the specific manufacturing process of the coated glass, if AZO is selected as the target material of the barrier layer, pure argon is used as the sputtering gas, and no reaction gas is added; if TiO is selectedxOr NiCrOxAs the target material of the barrier layer, a mixed gas of argon and oxygen is used as the sputtering gas, wherein the volume content of oxygen is less than or equal to 10%, preferably less than or equal to 7%. The sputtering power may be 10-40 kw.
The invention adopts the novel barrier technology of sputtering the metal oxide ceramic target by the direct current power supply, avoids the problem of the change of the absorption characteristic of the barrier layer before and after tempering, and is beneficial to preparing the low-emissivity coated glass with thermal stability. Meanwhile, the novel blocking technology adopts a direct-current power supply to sputter the rotating target, avoids the problems of arc striking or slag falling and the like of the ceramic target, and solves the technical problem of the AZO target in the actual production. In addition, the metal oxide barrier layer prepared by the process has the dual characteristics of metal and dielectric, and the barrier layer has low absorption to visible light, so that the metal oxide barrier layer can be used as a protective layer of a silver layer or a silver alloy layer and can also be used as a dielectric layer. Particularly, in the toughening process, the metal oxide barrier layer has a positive effect on the stability of the film structure and the color stability. Because the metal oxide barrier layer can not generate obvious optical property change when being heated, the metal oxide barrier layer can play a role in blocking oxygen and can effectively protect the silver layer from being damaged.
In one embodiment of the invention, the thicknesses of the first barrier layer, the second barrier layer and the third barrier layer are respectively controlled to be 0.5-5 nm, so that the high visible light transmittance of a product can be ensured, and the barrier effect is good.
In one embodiment of the invention, the first infrared reflective layer, the second infrared reflective layer and the third infrared reflective layer are silver or a silver alloy. Preferably, the first ir reflecting layer, the second ir reflecting layer and the third ir reflecting layer are silver alloy, the main component of the silver alloy is silver and comprises at least one element selected from the group consisting of gold, titanium, palladium, copper and niobium, wherein the at least one element selected from the group consisting of gold, titanium, palladium, copper and niobium is present in an amount of 0.3 to 10at.% based on the total amount of the silver alloy, wherein at.% means atomic percent. Compared with a pure silver layer, the silver alloy layer can obviously improve the moisture resistance and water vapor resistance of the silver-based low-radiation coated glass, prolong the oxidation resistance time of the coated glass and obviously reduce the white point defect of the silver-based low-radiation coated glass caused by the migration and aggregation of silver atoms in a film layer.
In one embodiment of the present invention, the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer each have a thickness of 5 to 15 nm. In a specific manufacturing process, a direct-current power supply and a planar cathode can be adopted to form the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer by sputtering deposition in an argon atmosphere. The power of the vacuum magnetron sputtering equipment can be 3-15 kw.
In one embodiment of the invention, the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are Si3N4、SnO2、Zn2SnO4、Nb2O5And ZnAlOxTwo or more kinds of combined film layer, wherein ZnAlOxRefers to aluminum doped zinc oxide (Aldoped-ZnO), in one embodiment ZnAlOxIn particular, 2 wt% of Al2O32 wt% aluminum doped zinc oxide (2 wt% Alded-ZnO). In a preferred embodiment, the first composite dielectric layer, the second composite dielectric layer and the third composite dielectric layer at least comprise a layer of 2 wt% of Aldoped-ZnO, and the layer is connected with the Ag film and positioned below the silver film, so that the preferred orientation growth of the subsequent silver film is facilitated, the surface resistance of the silver film is reduced, and the radiance of the whole silver-based low-emissivity film is further reduced.
In one embodiment of the invention, the thicknesses of the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are respectively 10-85 nm. The composite dielectric layer can effectively block Na ions diffused by the glass substrate during tempering or hot bending. In a specific manufacturing process, a first composite dielectric layer, a second composite dielectric layer, a third composite dielectric layer and a fourth composite dielectric layer can be formed by sputtering deposition under argon nitrogen or argon oxygen mixed atmosphere by adopting medium-frequency alternating voltage and a double-rotating cathode. The power of the vacuum magnetron sputtering equipment can be 10-60kw, and the frequency of the medium-frequency power supply can be 40 kHz.
In one embodiment of the invention, the coated glass further comprises a protective layer outside the fourth composite dielectric layer, and the protective layer is TiO2、Si3N4、SiNxOy(x/y > 1.3) or ZrO2At least one of (1) and (2) has a thickness of 5 to 30 nm. The protective layer enhances the scratch resistance and the wear resistance of the silver-based low-emissivity coated glass. In a specific manufacturing process, the protective layer can be formed by sputtering deposition under a mixed atmosphere of argon nitrogen or argon oxygen by adopting a medium-frequency alternating-current voltage and a double-rotating cathode. The power of the vacuum magnetron sputtering equipment can be 15-50kw, and the frequency of the medium-frequency power supply can be 40 kHz.
The following detailed description will explain the preparation process of the present invention and the performance advantages of the prepared coated glass by specific examples.
Example 1
The film structure of this example was Si from the glass substrate (6mm) outward in order3N4/Zn2SnO4/ZnAlOxAg alloy/TiOx/Zn2SnO4/ZnAlOxAg alloy/TiOx/Zn2SnO4/ZnAlOxAg alloy/TiOx/Zn2SnO4/Si3N4。
The processing technology and the parameters of the film layer are explained as follows:
background vacuum < 5X 10 for all chambers-5mbar, gas pressure of about 10 during sputtering-3mbar。
Sputtering a first, a second, a third and a fourth composite dielectric layers: adopts medium-frequency alternating voltage and a double-rotating cathode in mixed atmosphere (argon nitrogen or argon oxygen)) And (4) performing lower sputtering deposition, wherein the power of a vacuum magnetron sputtering device is 10-60kw, and the frequency of a medium-frequency power supply is 40 kHz. Wherein Si is prepared3N4A film layer, wherein a double-rotating cathode SiAl target (Si: Al is 90:10) is sputtered by adopting an intermediate frequency power supply, and the volume ratio of argon to nitrogen is kept at 1.2: 1; preparation of Zn2SnO4A film layer, which adopts mixed gas to reactively sputter ZnSn target (Zn: Sn: 50), and the argon-oxygen volume ratio is kept at 1: 1.2; preparation of ZnAlOxA film layer, which is reactively sputtered by alternating current cathode ZnAl (Zn: Al 98:2) with an argon-oxygen volume ratio of 1.3: 1.
Sputtering a first infrared reflecting layer, a second infrared reflecting layer and a third infrared reflecting layer: sputtering deposition is carried out by adopting a direct current power supply and a planar cathode in a pure argon atmosphere, and the power of a vacuum magnetron sputtering device is 3-15 kw. A silver alloy is used, the main component of which is silver and which comprises 0.3 at.% gold.
Sputtering a first barrier layer, a second barrier layer and a third barrier layer: the metal oxide ceramic target (rotary target) is prepared by sputtering a metal oxide ceramic Target (TiO) by adopting a direct-current power supplyx(x is more than or equal to 1.6 and less than or equal to 1.9), and the sputtering power is 10-40 kw. The sputtering gas is a mixed gas of argon and oxygen, the oxygen amount is low, and the volume ratio of argon to oxygen is kept at 15: 1.
Table 1 shows the film layer structure of this example and its material and thickness.
Table 1 film layer structure and film layer thickness of example 1
Table 2 shows the values of the color parameters before and after tempering, i.e. the characterization of the optical properties, for this example.
Table 2 optical properties of example 1
Note: tvis represents visible light transmittance; a and b represent a and b values of the transmission color respectively; rg represents the reflectivity of the glass surface, and a (Rg) and b (Rg) respectively represent a and b values in the reflection color of the glass surface; the delta Eab represents the color difference before and after tempering, and the formula is as follows:
from the results in table 2 above, it is clear that the coated glass of example 1 has a high visible light transmittance, Tvis 64% (before tempering), and good color stability before and after tempering, Δ Eab < 1.5.
Example 2
The film structure of this example was Si from glass (6mm) outward in order3N4/Zn2SnO4/ZnAlOxAg alloy/AZO/Zn2SnO4/ZnAlOxAg alloy/AZO/Zn2SnO4/ZnAlOxAg alloy/AZO/Zn2SnO4/Si3N4。
The processing technology and the parameters of the film layer are explained as follows:
background vacuum < 5X 10 for all chambers-5mbar, gas pressure of about 10 during sputtering-3mbar。
Sputtering a first, a second, a third and a fourth composite dielectric layers: the intermediate frequency alternating voltage and a double-rotating cathode are adopted for reactive sputtering deposition in mixed atmosphere (argon nitrogen or argon oxygen), the power of a vacuum magnetron sputtering device is 10-60kw, and the frequency of an intermediate frequency power supply is 40 kHz. Wherein Si is prepared3N4A film layer, wherein a double-rotating cathode SiAl target (Si: Al is 90:10) is sputtered by adopting an intermediate frequency power supply, and the volume ratio of argon to nitrogen is kept at 1.2: 1; preparation of Zn2SnO4A film layer, adopting mixed gas to reactively sputter ZnSn (Zn: Sn: 50), wherein the argon-oxygen volume ratio is kept at 1: 1.2; preparation of ZnAlOxFilm layer, by alternating current cathode reactive sputtering of ZnAl target (Zn: Al ═ 98:2), whichThe argon to oxygen volume ratio was maintained at 1.3: 1.
Sputtering a first infrared reflecting layer, a second infrared reflecting layer and a third infrared reflecting layer: sputtering deposition is carried out by adopting a direct-current power supply and a planar cathode in a pure argon atmosphere, and the power of a vacuum magnetron sputtering device is 3-15 kw. A silver alloy is used, the main component of which is silver and comprises 5 at.% titanium, palladium and copper.
Sputtering a first barrier layer, a second barrier layer and a third barrier layer: the metal oxide ceramic target is prepared by sputtering a metal oxide ceramic target (rotating target) by using a direct current power supply, wherein the metal oxide ceramic target is AZO (98 wt% ZnO:2 wt% Al)2O3) The sputtering power is 10-40 kw. The sputtering gas was pure argon.
Table 3 shows the film layer structure of this example and its materials and thicknesses.
Table 3 film layer structure and film layer thickness of example 2
Table 4 shows the values of the color parameters before and after tempering, i.e. the characterization of the optical properties, for this example.
Table 4 optical properties of example 2
From the results in Table 4 above, it is clear that the coated glass of example 2 has a visible light transmittance of 70.6% (before tempering), and a Δ Eab of less than 1.5 before and after tempering, and the color stability of the product is good.
Example 3
The film structure of this example was Si from glass (6mm) outward in order3N4/Zn2SnO4/ZnAlOxAg alloy/NiCrOx/Zn2SnO4/ZnAlOxAg alloy/NiCrOx/Zn2SnO4/ZnAlOxAg alloy/NiCrOx/Zn2SnO4/Si3N4。
The processing technology and the parameters of the film layer are explained as follows:
background vacuum < 5X 10 for all chambers-5mbar, gas pressure of about 10 during sputtering-3mbar。
Sputtering a first, a second, a third and a fourth composite dielectric layers: the intermediate frequency alternating voltage and a double-rotating cathode are adopted for sputtering deposition in mixed atmosphere (argon nitrogen or argon oxygen), the power of a vacuum magnetron sputtering device is 10-60kw, and the frequency of an intermediate frequency power supply is 40 kHz. Wherein Si is prepared3N4A film layer, wherein a double-rotating cathode SiAl target (Si: Al is 90:10) is sputtered by adopting an intermediate frequency power supply, and the volume ratio of argon to nitrogen is kept at 1.2: 1; preparation of Zn2SnO4A film layer, which adopts mixed gas to reactively sputter ZnSn target (Zn: Sn: 50), and the argon-oxygen volume ratio is kept at 1: 1.2; preparation of ZnAlOxA film layer, which is reactively sputtered by alternating current cathode ZnAl (Zn: Al 98:2) with an argon-oxygen volume ratio of 1.3: 1.
Sputtering a first infrared reflecting layer, a second infrared reflecting layer and a third infrared reflecting layer: sputtering deposition is carried out by adopting a direct current power supply and a planar cathode in a pure argon atmosphere, and the power of a vacuum magnetron sputtering device is 3-15 kw. A silver alloy is used, the main component of which is silver and comprises 10at.% titanium, palladium, copper and niobium.
Sputtering a first barrier layer, a second barrier layer and a third barrier layer: the metal oxide ceramic target (rotary target) is prepared by sputtering a metal oxide ceramic target (NiCrO) by adopting a direct-current power supplyx(x is more than or equal to 0.5 and less than or equal to 1) and the sputtering power is 10-40 kw. The sputtering gas is a mixed gas of argon and oxygen, the oxygen amount is low, and the volume ratio of argon to oxygen is kept at 100: 9.
Table 5 shows the film layer structure of this example and its materials and thicknesses.
Table 5 film layer structure and film layer thickness of example 3
Table 6 shows the values of the color parameters before and after tempering, i.e. the characterization of the optical properties, for this example.
TABLE 6 optical Properties of example 3
From the results of Table 6 above, it is clear that the coated glass of example 3 has a visible light transmittance of 67% (before tempering), and a Δ Eab of less than 1.5 before and after tempering, and the color stability of the product is good.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.
Claims (10)
1. The coated glass is characterized by comprising a glass substrate and a film layer formed on the glass substrate, wherein the film layer comprises the following components in sequence from the glass substrate to the outside: the infrared reflection film comprises a first composite dielectric layer, a first infrared reflection layer, a first barrier layer, a second composite dielectric layer, a second infrared reflection layer, a second barrier layer, a third composite dielectric layer, a third infrared reflection layer, a third barrier layer and a fourth composite dielectric layer, wherein the first barrier layer, the second barrier layer and the third barrier layer are prepared by sputtering a metal oxide ceramic target by a direct-current power supply, and the first barrier layer, the second barrier layer and the third barrier layer are prepared by sputtering a metal oxide ceramic target by using a direct-current power supplyThe metal oxide ceramic target is selected from AZO and TiOxOr NiCrOxAnd is a rotating target.
2. The coated glass according to claim 1, wherein the first barrier layer, the second barrier layer and the third barrier layer each have a thickness of 0.5 to 5 nm.
3. The coated glass of claim 1, wherein the first, second, and third infrared reflective layers are silver or a silver alloy;
preferably, the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer are silver alloy, the main component of the silver alloy is silver, and the silver alloy comprises at least one element selected from gold, titanium, palladium, copper and niobium, wherein the content of the at least one element selected from gold, titanium, palladium, copper and niobium accounts for 0.3 to 10at.% of the total amount of the silver alloy;
preferably, the thicknesses of the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer are respectively 5-15 nm.
4. The coated glass of claim 1, wherein the first, second, third and fourth composite dielectric layers are Si3N4、SnO2、Zn2SnO4、Nb2O5And ZnAlOxTwo or more combined film layers;
preferably, the thicknesses of the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are 10-85 nm respectively.
5. The coated glass of claim 1, further comprising a protective layer outside the fourth composite dielectric layer, wherein the protective layer is TiO2、Si3N4、SiNxOyOr ZrO2At least one of (a) and (b),the thickness is 5-30 nm.
6. A method of making the coated glass of any of claims 1-5, comprising: forming film layers in the following sequence from the glass substrate to the outside on the glass substrate through sputtering: the method comprises the steps of preparing a first composite dielectric layer, a first infrared reflecting layer, a first barrier layer, a second composite dielectric layer, a second infrared reflecting layer, a second barrier layer, a third composite dielectric layer, a third infrared reflecting layer, a third barrier layer and a fourth composite dielectric layer by sputtering a metal oxide ceramic target by a direct-current power supply, wherein the metal oxide ceramic target is selected from AZO, TiO and the likexOr NiCrOxAnd is a rotating target.
7. The method according to claim 6, wherein if AZO is selected as the target material of the barrier layer, pure argon is used as the sputtering gas without adding a reaction gas; if TiO is selectedxOr NiCrOxAs the target material of the barrier layer, a mixed gas of argon and oxygen is used as the sputtering gas, wherein the volume content of the oxygen is less than or equal to 10 percent, and preferably less than or equal to 7 percent;
preferably, the thicknesses of the first barrier layer, the second barrier layer and the third barrier layer are respectively 0.5-5 nm.
8. The method of claim 6, wherein the method comprises forming the first infrared reflective layer, the second infrared reflective layer, and the third infrared reflective layer by sputter deposition using a dc power source and a planar cathode under an argon atmosphere;
preferably, the thicknesses of the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer are respectively 5-15 nm;
preferably, the first infrared reflective layer, the second infrared reflective layer and the third infrared reflective layer are silver or silver alloy;
preferably, the first infrared reflecting layer, the second infrared reflecting layer and the third infrared reflecting layer are silver alloy, the main component of the silver alloy is silver, and the silver alloy comprises at least one element selected from gold, titanium, palladium, copper and niobium, wherein the content of the at least one element selected from gold, titanium, palladium, copper and niobium is 0.3 to 10at.% of the total amount of the silver alloy.
9. The method of claim 6, wherein the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are formed by sputtering deposition under argon-nitrogen or argon-oxygen mixed atmosphere by adopting medium-frequency alternating voltage and a double-rotating cathode;
preferably, the thicknesses of the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are respectively 10-85 nm;
preferably, the first composite dielectric layer, the second composite dielectric layer, the third composite dielectric layer and the fourth composite dielectric layer are Si3N4、SnO2、Zn2SnO4、Nb2O5And ZnAlOxTwo or more of them are combined into a film layer.
10. The method of claim 6, further comprising forming a protective layer outside the fourth composite dielectric layer by sputtering, the protective layer being TiO2、Si3N4、SiNxOyOr ZrO2At least one of (1) and (2), the thickness is 5-30 nm;
preferably, the method adopts intermediate frequency alternating current voltage and a double-rotating cathode to form the protective layer by sputtering deposition under the mixed atmosphere of argon nitrogen or argon oxygen.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109231847A (en) * | 2017-07-11 | 2019-01-18 | 中国南玻集团股份有限公司 | Half-reflection and half-transmission glass and preparation method thereof |
| CN108929045B (en) * | 2018-08-07 | 2021-04-16 | 江苏华玻光电技术有限公司 | Low radiation energy-saving glass and preparation method thereof |
| CN111138089A (en) * | 2018-11-06 | 2020-05-12 | 中国南玻集团股份有限公司 | Double silver glass |
| CN109336411A (en) * | 2018-12-05 | 2019-02-15 | 天津北玻玻璃工业技术有限公司 | A kind of high low radiation coated glass |
| CN110563344B (en) * | 2019-09-16 | 2022-05-27 | 传奇视界有限公司 | Energy-saving glass and preparation method and application thereof |
| CN110596981B (en) * | 2019-09-16 | 2022-04-19 | 传奇视界有限公司 | A kind of electrochromic glass with more neutral color tone and preparation method and application thereof |
| CN112624627A (en) * | 2019-10-08 | 2021-04-09 | 湖北亿钧耀能新材股份公司 | Automobile glass and manufacturing method thereof |
| CN112777945A (en) * | 2019-11-07 | 2021-05-11 | 中国南玻集团股份有限公司 | Three-silver glass |
| CN111733390A (en) * | 2019-12-30 | 2020-10-02 | 宁波瑞凌新能源科技有限公司 | Composite barrier material for double-reflection layer film and application thereof |
| CN111196683B (en) * | 2020-03-23 | 2025-01-21 | 中山市格兰特实业有限公司 | A kind of three-silver temperable three-property gray Low-E glass |
| CN111233345B (en) * | 2020-03-23 | 2024-08-13 | 中山市格兰特实业有限公司 | A super scratch-resistant triple-silver tempered Low-E glass |
| CN111253082B (en) * | 2020-03-23 | 2023-11-14 | 中山市格兰特实业有限公司 | A super-shielding and heat-insulating triple-silver temperable Low-E glass and its preparation method |
| CN111362590A (en) * | 2020-03-25 | 2020-07-03 | 四川猛犸半导体科技有限公司 | Thin film device |
| CN111517669A (en) * | 2020-06-09 | 2020-08-11 | 吴江南玻华东工程玻璃有限公司 | A kind of high-transmittance and low-reflection steel triple-silver low-emissivity glass and preparation method thereof |
| CN112194384A (en) * | 2020-10-26 | 2021-01-08 | 四川宇光光学玻璃有限公司 | Coated glass processing technology |
| CN113264691A (en) * | 2021-05-31 | 2021-08-17 | 天津耀皮工程玻璃有限公司 | High-weather-resistance coated glass and preparation method thereof |
| CN115849731A (en) * | 2021-09-26 | 2023-03-28 | 河北勒克斯光学薄膜技术有限公司 | Temperable glass mirror and preparation method thereof |
| CN113896432B (en) * | 2021-10-18 | 2024-03-12 | 上海玻光科技合伙企业(有限合伙) | Coated automobile glass |
| CN114044632A (en) * | 2021-12-16 | 2022-02-15 | 西湖大学 | Vehicle glass and preparation method thereof |
| CN116514409A (en) * | 2022-12-15 | 2023-08-01 | 天津南玻节能玻璃有限公司 | A kind of medium and low permeability steel low-emissivity coated glass |
| CN119898088A (en) * | 2024-04-01 | 2025-04-29 | 江苏城乡建设职业学院 | A dynamically adjusted coated glass, and a preparation method and a detection method thereof |
| CN119774892A (en) * | 2024-12-31 | 2025-04-08 | 天津南玻节能玻璃有限公司 | A low-transmittance and low-reflection coated glass |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6495263B2 (en) * | 1999-12-06 | 2002-12-17 | Guardian Industries Corp. | Low-E matchable coated articles and methods of making same |
| CN102372447B (en) * | 2010-08-24 | 2014-05-07 | 中国南玻集团股份有限公司 | Low emissivity glass containing silver and manufacture method |
| CN103879080A (en) * | 2012-12-21 | 2014-06-25 | 中国南玻集团股份有限公司 | Three-silver-layer low-radiation glass and preparation method thereof |
| CN104325736A (en) * | 2014-10-30 | 2015-02-04 | 中山市亨立达机械有限公司 | Three-silver LOW-E coated glass |
-
2015
- 2015-05-26 CN CN201510275011.5A patent/CN105152549A/en active Pending
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| CN105152549A (en) | 2015-12-16 |
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