CN101224952B - On-line preparation method of surface graded oxidation low-reflection nano-silicon coated glass - Google Patents

On-line preparation method of surface graded oxidation low-reflection nano-silicon coated glass Download PDF

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Publication number
CN101224952B
CN101224952B CN2008100598448A CN200810059844A CN101224952B CN 101224952 B CN101224952 B CN 101224952B CN 2008100598448 A CN2008100598448 A CN 2008100598448A CN 200810059844 A CN200810059844 A CN 200810059844A CN 101224952 B CN101224952 B CN 101224952B
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coated glass
nano
annealing furnace
silicon coated
silicon
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CN101224952A (en
Inventor
韩高荣
杜丕一
宋晨路
翁文剑
刘涌
赵高凌
沈鸽
徐刚
张溪文
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses an online method for preparing low-reflection nano-silicon coated glass with a gradient oxidized surface. The nano-silicon coated glass formed on line in a tin channel on the production line of float glass is continuously sent into an annealing furnace and is heat-treated under constant temperature for 1-3 minutes in high-temperature area of the annealing furnace so as to prepare the low-reflection nano-silicon coated glass with a gradient oxidized surface. The low-reflection nano-silicon coated glass with the gradient oxidized surface prepared through the method of the invention has reflectivity below 15 percent, thus effectively reducing optical pollution to the environment during the application of the coated glass.

Description

The online preparation method of surface graded oxidation low-reflection nano-silicon coated glass
Technical field
The present invention relates to the technology of preparing and the Application Areas thereof of composite film coating glass, especially, relate to a kind of online preparation method of surface graded oxidation low-reflection nano-silicon coated glass.
Background technology
Early stage sunlight controlling coated glass normally forms (these coated glasses are mainly with the method preparation of off-line) by being coated with metal such as Au, Ti, Ag and metallic compound film at glass surface, its surface has very strong specular reflection, that its specular reflectance has even up to 60~70%, thereby easily bring so-called " light pollution " problem to surrounding environment.The coated glass of online preparation is a kind of energy-saving high-performance coated glass, particularly nano-silicon coated glass can reach below 40% usually owing to the higher uptake factor of its Nano thin film makes the sunlight controlling coated glass specular reflection of making thus less relatively.But along with the continuous progress of society and the enhancing of environmental consciousness, environmental protection requirement is improved constantly thereupon, nowadays the reflectivity that clearly is defined in traffic main artery and its buildings of turning road junction in new traffic support regulations must be lower than 16%, and in the ordinary course of things, its specular reflectance also should be less than 30%, guaranteeing that people do not have dazzling sensation, thereby it is imperative further to develop the coated glass of ultralow reflectivity.Prepare more high performance film and coated glass and become the essential of energy-saving glass field.
The combination film optical computing, analyzed transmission, refraction and the reflection process of specific refractory power to going into to inject rete light in the rete, if design calculation is found rete when existing with a plurality of thin layers of specific refractory power continually varying, this rete is very obvious to the influence of input path, if also be the rete multi-layer compound film that from outward appearance to inner essence increases gradually of specific refractory power from level to level, the maximized decline of reflection of incident light rate meeting can reach antireflecting purpose.As seen,, then can reduce the specular reflectance of coated glass greatly, the preparation low-reflection plating glass if in the rete of coated glass, be designed to the multilayer film that refractive index gradient changes.But, the characteristics of coated glass are dynamically produced in consideration on float glass process online production technology, how original single thin film being prepared into the multilayer film that specific refractory power gradually changes will become the very big difficult point that makes a breakthrough and succeed, and also be the key that obtains ultralow reflection coated glass.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of online preparation method of surface graded oxidation low-reflection nano-silicon coated glass is provided.
The objective of the invention is to be achieved through the following technical solutions: a kind of online preparation method of surface graded oxidation low-reflection nano-silicon coated glass, the nano-silicon coated glass of online formation in the molten tin bath on the float glass process line is sent into annealing furnace continuously, carried out constant temperature thermal treatment 1~3 minute in the annealing furnace high-temperature zone, the preparation surface graded oxidation low-reflection nano-silicon coated glass.
Further, in the described annealing furnace, the oxygen volume is 22%~60% of total gas volume; The temperature distribution of annealing furnace is: the ingress temperature is the highest, and it is suitable with the tin bath outlet temperature, is controlled at 580~630 ℃; The exit temperature is minimum, is controlled at below 100 ℃; Described nano-silicon coated glass movement velocity is 360~545 meters/hour.
The invention has the beneficial effects as follows: the online preparation method of surface graded oxidation low-reflection nano-silicon coated glass of the present invention is directly in conjunction with the annealing furnace that utilizes in the float glass process, reinforcement diffusion process by oxygen, nano-silicon coated glass in the continuous traveling process has been realized online superficial film graded oxidation, obtained superficial film and had the low-reflection plating glass that graded index changes.
Embodiment
Describe the present invention in detail according to embodiment below, it is more obvious that purpose of the present invention and effect will become.
Theoretically analog calculation is carried out in the formation of surperficial graded index, combined process and silicon film characteristics, design utilizes the oxidation of surface silicon to form the low-refraction silicon oxide and produces the gradient layer of silicon oxide, can clearly be seen that the reflectivity of this Nano thin film through surface graded oxidation will descend greatly.Based on this notional result, diffusion is strengthened in exploitation and continuous alternating temperature is controlled to the online graded oxidation new technology of film surface layer, at nano-silicon coated glass, and in conjunction with existing float glass equipment characteristic, design utilizes annealing furnace at high temperature to carry out the reinforcement diffusion of oxygen after glass leaves molten tin bath and controls continuous alternating temperature thermal treatment, is formed on the Nano thin film upper layer with this and has the energy-conservation coated glass of novel ultralow reflection nano-silicon that graded index changes.Successfully realized and obtained surface graded oxidation low-reflection nano-silicon coated glass at present.
This method specific as follows: the nano-silicon coated glass of online formation in the molten tin bath on the existing float glass process line is sent into annealing furnace continuously, carried out constant temperature thermal treatment 1~3 minute in the annealing furnace high-temperature zone, the preparation surface graded oxidation low-reflection nano-silicon coated glass; By oxygen volume in the annealing furnace is 22%~60% of total gas volume; The temperature distribution of annealing furnace is: the ingress temperature is the highest, and it is suitable with the tin bath outlet temperature, is controlled at 580~630 ℃, and the exit temperature is minimum, remains on below 100 ℃, and it is 1~1.003 normal atmosphere that annealing furnace is strengthened spreading area glass surface air pressure; The glass movement velocity is 360~545 meters/hour.The graded oxidation layer thickness is about 25~40nm in the film of the surface graded oxidation low-reflection nano-silicon coated glass of preparation, and from outward appearance to inner essence oxygen level reduces gradually.
This method is suitable for the coated glass of online preparation graded oxidation non-crystalline silicon (carbon, nitrogen) film, nano-silicon/nanometer silicon carbide, nano-silicon/nano-silicon nitride, non-crystalline silicon/nano-silicon/nanometer silicon carbide, non-crystalline silicon/nano-silicon/nano-silicon nitride and non-crystalline silicon/nano-silicon/nanometer silicon carbide/nano silicon nitride composited film equally.
Specific embodiment is as follows:
Embodiment 1
On the float glass process line in the molten tin bath nano-silicon coated glass of online formation send into annealing furnace continuously with 360 meters/hour, oxygen content is 25% of total gas volume in the control annealing furnace, annealing furnace ingress temperature is controlled at 620 ℃, the exit temperature remains on below 100 ℃, glass enters to be controlled it in the high-temperature zone behind the annealing furnace and carries out constant temperature thermal treatment, 1 minute time, it is 1 normal atmosphere that diffusion zone glass surface air pressure is strengthened in control, the coated glass superficial film of preparation has graded index, and coated glass surface specular reflectance is 14.5%.
Embodiment 2
On the float glass process line in the molten tin bath nano-silicon coated glass of online formation send into annealing furnace continuously with 450 meters/hour, oxygen content is 45% of total gas volume in the control annealing furnace, annealing furnace ingress temperature is controlled at 600 ℃, the exit temperature remains on below 100 ℃, glass enters to be controlled it in the high-temperature zone behind the annealing furnace and carries out constant temperature thermal treatment, 2 minutes time, it is 1.001 normal atmosphere that diffusion zone glass surface air pressure is strengthened in control, the coated glass superficial film of preparation has graded index, and coated glass surface specular reflectance is 13.8%.
Embodiment 3
On the float glass process line in the molten tin bath nano-silicon coated glass of online formation send into annealing furnace continuously with 540 meters/hour, oxygen content is 60% of total gas volume in the control annealing furnace, annealing furnace ingress temperature is controlled at 580 ℃, the exit temperature remains on below 100 ℃, glass enters to be controlled it in the high-temperature zone behind the annealing furnace and carries out constant temperature thermal treatment, 3 minutes time, it is 1.003 normal atmosphere that diffusion zone glass surface air pressure is strengthened in control, the coated glass superficial film of preparation has graded index, and coated glass surface specular reflectance is 14.1%.

Claims (1)

1. the online preparation method of a surface graded oxidation low-reflection nano-silicon coated glass, it is characterized in that, the nano-silicon coated glass of online formation in the molten tin bath on the float glass process line is sent into annealing furnace continuously, carried out constant temperature thermal treatment 1~3 minute in the annealing furnace high-temperature zone, the preparation surface graded oxidation low-reflection nano-silicon coated glass; In the described annealing furnace, the oxygen volume is 22%~60% of total gas volume; The temperature distribution of described annealing furnace is: the ingress temperature is the highest, and it is suitable with the tin bath outlet temperature, is controlled at 580~630 ℃; The exit temperature is minimum, is controlled at below 100 ℃; Described nano-silicon coated glass movement velocity is 360~545 meters/hour.
CN2008100598448A 2008-02-19 2008-02-19 On-line preparation method of surface graded oxidation low-reflection nano-silicon coated glass Expired - Fee Related CN101224952B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607175A (en) * 1967-11-09 1971-09-21 Pilkington Brothers Ltd Control system for modifying the surface of float glass
CN1167003A (en) * 1996-05-30 1997-12-10 三菱重工业株式会社 Method for treating fume and system thereof
EP1034146B1 (en) * 1997-11-04 2002-08-21 Pilkington Plc Improvements in coating glass
CN1899998A (en) * 2006-07-18 2007-01-24 福耀集团双辽有限公司 Method and device for online coating flat glass

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607175A (en) * 1967-11-09 1971-09-21 Pilkington Brothers Ltd Control system for modifying the surface of float glass
CN1167003A (en) * 1996-05-30 1997-12-10 三菱重工业株式会社 Method for treating fume and system thereof
EP1034146B1 (en) * 1997-11-04 2002-08-21 Pilkington Plc Improvements in coating glass
CN1899998A (en) * 2006-07-18 2007-01-24 福耀集团双辽有限公司 Method and device for online coating flat glass

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JP特开平8-231232A 1996.09.10
刘起英等.低辐射镀膜玻璃的现状及展望.《玻璃》.2002,(第6期),9-13. *

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Application publication date: 20080723

Assignee: Weihai Blue Star Glass Group Co., Ltd.

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Denomination of invention: On-line preparation method of surface graded oxidation low-reflection nano-silicon coated glass

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