CN103753896B - Lanthanum-boride-doped AZO (aluminum-doped zinc oxide) low-emissivity coated glass and preparation method thereof - Google Patents

Abstract

The invention provides a lanthanum-boride-doped AZO (aluminum-doped zinc oxide) low-emissivity coated glass which comprises a glass substrate and a coating layer, wherein the coating layer sequentially comprises a first layer TiOx, a second layer LaB6-AZO, a third layer Ag, a fourth layer NiCr, a fifth layer LaB6-AZO and a sixth layer Si3N4 from inside to outside. The invention also provides a preparation method of the coated glass. The coated glass has the advantages of higher visible light transmittance (3-4% higher than AZO); in the low-emissivity product, the Ag used as the bottom layer has better binding force with Ag; the product has the advantages of low emissivity, stable performance and stable optical and thermal properties; and the method is suitable for large-scale production. The glass has the characteristics of favorable appearance color, low tendency to shedding of the coating and the like, and can be used in an interlayer or hollow mode.

Description

A kind of doping lanthanum boride AZO low radiation coated glass and preparation method thereof

Technical field

The present invention relates to a kind of coated glass, relate to a kind of doping lanthanum boride AZO low radiation coated glass and preparation method thereof more specifically.

Background technology

At present, the application of transparent dielectric film in large-area coating film glass is very extensive.Wherein, ceramic state zinc oxide aluminum (AZO) due to sputter rate fast, pure Ar can be used to sputter, and sputtering condition is easily controlled, and can save trapping target position and film visible light-transmissive advantages of higher and obtain extensive Study and appliance.But ceramic state AZO target is after installing and using a period of time, and dross electric discharge phenomena easily appear in surface, have a strong impact on use power and the life-span of target, coated product also can have been caused to there is the hidden danger of colour fluctuation simultaneously.AZO rete is as the easy demoulding of prime coat of Ag.

Summary of the invention

The object of the invention is the technological deficiency for prior art, the present invention aims to provide a kind of low radiation coated glass, for realizing above technical goal, the present invention is by the following technical solutions: a kind of doping lanthanum boride AZO low radiation coated glass, comprise glass substrate and film plating layer, film plating layer comprises from inside to outside successively: ground floor TiOx, the second layer: LaB ₆-AZO, third layer: Ag, the 4th layer: NiCr, layer 5: LaB ₆-AZO, layer 6: Si ₃n ₄, second layer Ag prime coat is LaB ₆-AZO.

Further, described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 2.5 ~ 10wt%.

A kind of doping lanthanum boride AZO low radiation coated glass, ground floor TiOx thickness is 15 ~ 25nm, the second layer: LaB ₆-AZO thickness is 20 ~ 30nm, third layer: Ag thickness be 5 ~ 15nm, the 4th layer: NiCr thickness 1 ~ 5nm, layer 5: LaB ₆-AZO thickness 15 ~ 25nm, layer 6: SiNx thickness 20 ~ 45nm.

Adulterate the preparation method of lanthanum boride AZO low radiation coated glass, comprises the steps:

(1) acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate is successively used;

(2) dry;

(3) put into vacuum chamber to vacuumize;

(4) be filled with 1200sccm pure Ar gas sputtering ceramic alumina titanium target after reaching vacuum to carry out target table and clean, after 5min, the preparation of TiOx film is carried out in straight argon sputtering;

(5) close this target after reaching thickness, straight argon carries out the clean and doping LaB of target table successively ₆aZO target, Ag target, NiCr target and top layer LaB ₆aZO rete;

(6) carry out target table with pure Ar to clean, then use Ar:N ₂for the mist Slag coating SiNx film of 1:1.6.

Doping lanthanum boride AZO low radiation coated glass light-plated mathematic(al) parameter is: LaB ₆-AZO film is 1.75 ~ 2.1 in the refractive index of 550nm place light wave, and extinction coefficient is about 0.

Glass substrate thickness of the present invention comprises: 4,5,6,8,10,12,15,19mm.Glass colour comprises: ultrawhite glass, white glass, green glass, grey glass, crystal ash glass, blue glass, ocean blue glass, dark-brown glass etc.Glass structure comprises: laminated glass, colored glazed glass, safety glass, semi-tempered glass, annealed glass, flame resistant glass, double glazing etc.

Coated glass of the present invention has the following advantages:

1. this coated product visible light transmissivity is higher, and the relative AZO of transmitance can improve 3 ~ 4%;

2. this film surface is more smooth, in Low-E product, as the prime coat of Ag and the adhesion of Ag better;

3. the radiance of this film layer is than the LaB that do not adulterate ₆aZO radiance low;

4. properties of product are stablized, and are suitable for large-scale production, and optics and thermal property are stablized.The features such as this glass has good appearance color, rete difficult drop-off.Can interlayer or the use of conjunction hollow.

Accompanying drawing explanation

Fig. 1 adulterates lanthanum boride AZO low radiation coated glass structural representation

Fig. 2 glass surface reflectance spectrum

Fig. 3 face reflectance spectrum

Fig. 4 is through spectrum

Detailed description of the invention

In order to illustrate technical scheme of the present invention and technical purpose, below in conjunction with the drawings and the specific embodiments, the present invention is described further.

Embodiment 1

A kind of doping lanthanum boride AZO low radiation coated glass, comprise glass substrate and film plating layer, film plating layer comprises from inside to outside successively: ground floor TiOx, the second layer: LaB ₆-AZO, third layer: Ag, the 4th layer: NiCr, layer 5: LaB ₆-AZO, layer 6: Si ₃n ₄, second layer Ag prime coat is LaB ₆-AZO.

Ground floor TiOx thickness is 20nm, second layer LaB ₆-AZO thickness is 24nm, third layer Ag thickness is 6nm, the 4th layer of NiCr thickness 1.9nm, layer 5 LaB ₆-AZO thickness 18nm, layer 6 SiNx thickness 30nm.

Described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 5wt%.

Embodiment 2

A kind of doping lanthanum boride AZO low radiation coated glass, comprise glass substrate and film plating layer, film plating layer comprises from inside to outside successively: ground floor TiOx, the second layer: LaB ₆-AZO, third layer: Ag, the 4th layer: NiCr, layer 5: LaB ₆-AZO, layer 6: Si ₃n ₄, second layer Ag prime coat is LaB ₆-AZO.

Ground floor TiOx thickness is 12nm, second layer LaB ₆-AZO thickness is 30nm, third layer Ag thickness is 15nm, the 4th layer of NiCr thickness 3nm, layer 5 LaB ₆-AZO thickness 25nm, layer 6 SiNx thickness 20nm.

Described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 10wt%.

Embodiment 3

A kind of doping lanthanum boride AZO low radiation coated glass, comprise glass substrate and film plating layer, film plating layer comprises from inside to outside successively: ground floor TiOx, the second layer: LaB ₆-AZO, third layer: Ag, the 4th layer: NiCr, layer 5: LaB ₆-AZO, layer 6: Si ₃n ₄, second layer Ag prime coat is LaB ₆-AZO.

Ground floor TiOx thickness is 25nm, second layer LaB ₆-AZO thickness is 20nm, third layer Ag thickness is 10nm, the 4th layer of NiCr thickness 5nm, layer 5 LaB ₆-AZO thickness 15nm, layer 6 SiNx thickness 45nm.

Described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 2.5wt%.

Embodiment 4

The preparation process of above-mentioned coated glass is:

(1) acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate is successively used;

(2) dry;

(3) put into vacuum chamber to vacuumize;

(4) be filled with 1200sccm pure Ar gas sputtering ceramic alumina titanium target after reaching vacuum to carry out target table and clean, after 5min, the preparation of TiOx film is carried out in straight argon sputtering;

(5) close this target after reaching thickness, straight argon carries out the clean and doping LaB of target table successively ₆aZO target, Ag target, NiCr target and top layer LaB ₆aZO rete;

(6) carry out target table with pure Ar to clean, then use Ar:N ₂for the mist Slag coating SiNx film of 1:1.6.

Embodiment 5

As shown in Figure 2-4: the spectrogram of the coated glass of embodiment 1.

Glass surface reflection Rg:4.54, glass surface brightness L*g:61.04, face color value a*g:1.83, b*g:-1.86.Above-mentioned color is optimum color, and reality is every can deviation 0.8.

Face reflection Rf:6.34, face brightness L*f:30.25, face color value a*f:1.84, b*f:9.58.Above-mentioned color is optimum color, and reality is every can deviation 0.8.

Glass through T:77.29, through brightness L*t:90.45, color coordinates a*t:-1.7, b*t:-2.04.Above-mentioned color is optimum color, and reality is every can deviation 0.8.

Above embodiments of the invention have been described in detail, but described content is only preferred embodiment of the present invention, not in order to limit the present invention.All make in application range of the present invention any amendment, equivalent to replace and improvement etc., all should be included within protection scope of the present invention.

Claims (7)

1. adulterate a lanthanum boride AZO low radiation coated glass, and it is characterized in that, comprise glass substrate and film plating layer, film plating layer comprises from inside to outside successively: ground floor: TiO _x, the second layer: LaB ₆-AZO, third layer: Ag, the 4th layer: NiCr, layer 5: LaB ₆-AZO, layer 6: Si ₃n ₄.

2. a kind of doping lanthanum boride AZO low radiation coated glass according to claim 1, is characterized in that, described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 2.5 ~ 10wt%.

3. a kind of doping lanthanum boride AZO low radiation coated glass according to claim 1, is characterized in that, described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 3 ~ 8wt%.

4. a kind of doping lanthanum boride AZO low radiation coated glass according to claim 1, is characterized in that, described LaB ₆-AZO layer adopts vacuum magnetic-control sputtering method directly to sputter and mixes LaB ₆aZO target material, wherein LaB ₆incorporation is 4 ~ 6wt%.

5. a kind of doping lanthanum boride AZO low radiation coated glass according to claim 1, is characterized in that: ground floor TiO _xthickness is 15 ~ 25nm, the second layer: LaB ₆-AZO thickness is 20 ~ 30nm, third layer: Ag thickness be 5 ~ 15nm, the 4th layer: NiCr thickness 1 ~ 5nm, layer 5: LaB ₆-AZO thickness 15 ~ 25nm, layer 6: Si ₃n ₄thickness 20 ~ 45nm.

6. a kind of doping lanthanum boride AZO low radiation coated glass according to claim 5, is characterized in that, ground floor TiO _xthickness is 20nm, the second layer: LaB ₆-AZO thickness is 24nm, third layer: Ag thickness be 6nm, the 4th layer: NiCr thickness 1.9nm, layer 5: LaB ₆-AZO thickness 18nm, layer 6: Si ₃n ₄thickness 30nm.

7. the preparation method of a kind of lanthanum boride AZO low radiation coated glass that adulterates according to claim 6, it is characterized in that, wherein processing method is:

(1) acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate is successively used;

(2) dry;

(3) put into vacuum chamber to vacuumize;

(4) be filled with 1200sccm pure Ar gas sputtering ceramic alumina titanium target after reaching vacuum to carry out target table and clean, after 5min, TiO is carried out in straight argon sputtering _xthe preparation of film;

(5) close this target after reaching thickness, straight argon carries out the clean and doping LaB of target table successively ₆aZO target, Ag target, NiCr target and top layer LaB ₆aZO rete;

(6) carry out target table with pure Ar to clean, then use Ar:N ₂for the mist Slag coating Si of 1:1.6 ₃n ₄film.