CN104310798B - Preparation method of thermotropic reflective infrared coated glass - Google Patents
Preparation method of thermotropic reflective infrared coated glass Download PDFInfo
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- CN104310798B CN104310798B CN201410534503.7A CN201410534503A CN104310798B CN 104310798 B CN104310798 B CN 104310798B CN 201410534503 A CN201410534503 A CN 201410534503A CN 104310798 B CN104310798 B CN 104310798B
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Abstract
The invention discloses a preparation method of thermotropic reflective infrared coated glass. The method comprises the following steps: plating a silicon dioxide isolating layer on a high boron silicon glass substrate by adopting a magnetron sputtering method; plating a metal vanadium film layer on the isolating layer by adopting the magnetron sputtering method; using vanadium metal or tungsten doped vanadium metal as a target; plating a silicon dioxide on an infrared reflective layer by adopting the magnetron sputtering method as an antireflection layer to obtain the coated glass; and carrying out thermal treatment in an atmospheric environment and at a spatial temperature of 600-750 DEG C, wherein the metal vanadium film layer is oxidized to form the infrared reflective layer and meanwhile, the coated glass is tempered. The method is simple in preparation process, mature and free from pollution in the preparation process. The thermal treatment of the film layer of the obtained coated glass and the coated glass tempering are accomplished at one time, so that infrared rays can be reflected, visible light reflection is reduced, and the thermal shock resistance of the glass is improved.
Description
Technical field
The invention belongs to technical field of composite preparation, be specifically related to the preparation method of a kind of thermic reflection infrared ray coated glass.
Summary of the invention
Short-term or long-range circumstances are needed in household electrical appliances, household, kitchen oven and baking oven, locomotive and steamer glass pane and building etc.
Temperature uses the field of glass more than 200 DEG C～500 DEG C, due to simple glass transmission with absorb solar spectrum, including visible ray and
Closely, middle infrared (Mid-IR), adversely affect to the occasion of some specific use glass.Absorb infrared ray and cause glass temperature rise, expansion
Explosion, even Glass Transition lose intensity；Transmission infrared ray makes heat flow to low-temperature space from high-temperature region, causes energy loss.Example
As: the sight glass of baking box, it is generally required to stand 300 DEG C～500 DEG C, common float glass or common float glass process safety glass
The thermal shock of this temperature range can not be stood for a long time.Although the high-boron-silicon glass of low bulk is amenable to this temperature shock, but he is not
Can effectively stop heat to transmit, cause energy loss.
In order to overcome glass transmission heat to cause energy loss, glass swelling to cause glass explosion and temperature rise to cause Glass Transition to lose
The shortcoming going intensity, it is necessary to a kind of reflect infrared ray, low bulk, glass that glass transition temperature is high.This glass can lead to
Cross be coated with on high-boron-silicon glass thermic reflection infrared ray realize.
Thermic reflection infrared ray, it is simply that regulate and control whether to reflect infrared ray according to glass local environment temperature or glass temperature.
Vanadium dioxide is a kind of metal-oxide with phase transition property, and its phase transition temperature is 68 DEG C, the change of the forward and backward structure of phase transformation
Change cause its produce to infrared light by transmission to reflection reversible transition.But, this to reflecting ultrared transformation, also can make
Transmission of visible light declines.Theoretical according to Film Optics, the method reducing glass-reflected light is exactly plating one layer low on the glass surface
Deielectric-coating in glass refraction.
At present, the method being coated with thin film on glass mainly has sputtering method, vapour deposition method, wet chemistry method, wherein ripe magnetic control to spatter
Shooting method plated film, has that film uniformity is good, thicknesses of layers is easy to control, film layer is combined with glass and the feature such as pollution-free,
It is widely applied in the field producing coated glass.
Summary of the invention
The present invention provides the preparation method of a kind of thermic reflection infrared ray coated glass, along with temperature raises, reflects infrared ray, both
Stop heat transmission, again delay glass temperature rise.It may be used for baking box, building glass, locomotive and the heat-resisting sight glass of steamer etc.
Field.
For reaching above-mentioned purpose, use technical scheme as follows:
The preparation method of a kind of thermic reflection infrared ray coated glass, comprises the following steps:
1) magnetically controlled sputter method is used to be coated with silicon dioxide sealing coat on high-boron-silicon glass substrate；
2) magnetically controlled sputter method is used to be coated with vanadium metal film layer on sealing coat；With vanadium metal or witch culture vanadium metal as target；
3) use magnetically controlled sputter method to be coated with silicon dioxide film on infrared-reflecting layers and obtain coated glass as antireflection layer；
4) heat treatment at atmospheric environment, space temperature 600～750 DEG C, the oxidation of described vanadium metal film layer forms infrared-reflecting layers,
Coated glass is by tempering simultaneously.
By such scheme, described silicon dioxide sealing coat is 10～15nm.
By such scheme, described infrared reflection layer thickness is 20-60nm.
By such scheme, described silicon dioxide antireflection layer thicknesses of layers is 70～125nm.
By such scheme, the doping of described witch culture vanadium metal is 0-3.5wt%.
By such scheme, described thermic reflection infrared ray coated glass is for heat-resisting sight glass.
This invention takes magnetron sputtering method under room temperature on high-boron-silicon glass, be coated with multilayer film, utilize the phase transformation of vanadium dioxide film
Reflection infrared ray and the low-index film with vanadium dioxide film refractive index match reduce visible reflectance/increase visible ray
Absorbance.The coefficient of expansion of high-boron-silicon glass is little, it is possible to stand 300 DEG C～the thermal shock of 500 DEG C, minimizing glass explosion probability；
When ambient temperature reaches uniform temperature, coated glass reflection infrared ray makes glass extend temperature rising-time, postpone glass to softening point
Time, glass is made to have mechanical strength；Phase-change film layer reduces heat transmission, stops energy to run off or enters；Antireflection film layer makes
Glass vision panel becomes apparent from.This coated glass reaches film layer heat treatment by tempering simultaneously and increases the purpose of strength of glass.Formed
Even film layer and glass are firmly combined with, hardness, wearability and heat shock resistance reach real requirement thermic reflection infrared ray, can
See light antireflective bifunctional coated glass.Can be used for heatproof, heat insulation sight glass, such as: baking box glass, build heat-resisting every
Disconnected glass, locomotive and steamer etc. use the field of glass.
The beneficial effects of the present invention is:
Preparation technology is simple, method is ripe；
Preparation process is pollution-free；
The film layer heat treatment of the coated glass obtained once completes with coated glass tempering, it is possible to reflection infrared ray, minimizing visible ray
Reflection, improves the heat shock resistance of glass.
Detailed description of the invention
Following example explain technical scheme further, but not as limiting the scope of the invention.
The preparation method of thermic of the present invention reflection infrared ray coated glass, preparation process is as follows:
1) magnetically controlled sputter method is used to be coated with silicon dioxide sealing coat on high-boron-silicon glass substrate；
2) magnetically controlled sputter method is used to be coated with vanadium metal film layer on sealing coat；With vanadium metal or witch culture vanadium metal as target；
3) use magnetically controlled sputter method to be coated with silicon dioxide film on infrared-reflecting layers and obtain coated glass as antireflection layer；
4) heat treatment at atmospheric environment, space temperature 600～750 DEG C, the oxidation of described vanadium metal film layer forms infrared-reflecting layers,
Coated glass is by tempering simultaneously.
Optimally, silicon dioxide sealing coat is 10～15nm.
Optimally, infrared reflection layer thickness is 20-60nm.
Optimally, silicon dioxide antireflection layer thicknesses of layers is 70～125nm.
Optimally, the doping of witch culture vanadium metal is 0-3.5wt%.
Optimally, thermic reflection infrared ray coated glass is for heat-resisting sight glass.Such as: baking box glass, build heat-resisting partition
Glass, locomotive and steamer etc..
Optimally, high-boron-silicon glass substrate pretreatment to be coated: high-boron-silicon glass substrate deionized water to be coated is carried out clearly
Wash, be dried, obtain cleaned glass；Cleaned glass is put in the vacuum chamber of sputter coating, under normal pressure nitrogen divides, with 1100～
The Cement Composite Treated by Plasma glass surface that 1300V voltage is formed；Then the air pressure of vacuum chamber is extracted into 3.5～8.5*10-4Pa。
Embodiment 1
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 5%, sputtering pressure 2.5*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 10nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, argon is worked gas, sputtering pressure 2.5*10-1Pa, uses vanadium metal
Do target, be coated with the deposition on glass vanadium metal film of sealing coat, the thicknesses of layers 20nm of deposition.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 5%, sputtering pressure 2.5*10-1Pa reactive sputtering sinks
Long-pending high refractive index film/silicon dioxide film composite film, thicknesses of layers 70nm.
4, the coated glass obtained is heat treatment/tempering at atmospheric environment space temperature 600～750 DEG C, and vanadium metal film layer etc. is by warm
Reason is oxidized to vanadium dioxide, and coated glass is by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 45%；Reach in glass ambient temperature
To 70 DEG C, 2500nm wavelength infrared reflection rate 45%；Film hardness 5.5H～6.5H；Coated glass stands 1000 times 300
DEG C～the thermal shock in 3.5 hours of 500 DEG C of heat radiations.
Embodiment 2
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 10%, sputtering pressure 3.5*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 15nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, argon is worked gas, sputtering pressure 3.5*10-1Pa, uses witch culture
Vanadium metal is target (witch culture amount: percentage by weight 0.5%), the thicknesses of layers 20nm of deposition.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 5%, sputtering pressure 2.5*10-1PA reactive sputtering sinks
Long-pending high refractive index film/silicon dioxide film composite film, thicknesses of layers 70nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and witch culture vanadium film layer is heat-treated oxidation
Become vanadium dioxide, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 45%；Reach in glass ambient temperature
57 DEG C, 2500nm wavelength infrared reflection rate 50%；Film hardness 5.5H～6.5H；Coated glass stand 1000 times 300 DEG C～
The thermal shock in 3.5 hours of 500 DEG C of heat radiations.
Embodiment 3
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 10%, sputtering pressure 3.0*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 15nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, argon is worked gas, sputtering pressure 3.0*10-1Pa, uses witch culture
Vanadium metal is target (witch culture amount: percentage by weight 1.5%), the thicknesses of layers 40nm of deposition.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 10%, sputtering pressure 3.0*10-1Pa reactive sputtering
Deposit high refractive index film/silicon dioxide film composite film, thicknesses of layers 90nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and witch culture vanadium film layer is heat-treated oxidation
Become vanadium dioxide, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 50%；Glass ambient temperature from
43 DEG C of beginnings, coated glass is to 2500nm wavelength infrared reflection rate 50%；Film hardness 6.0H；Coated glass stands 1000
Secondary 300 DEG C～the thermal shock in 3.5 hours of 500 DEG C of heat radiations.
Embodiment 4
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 15%, sputtering pressure 3.5*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 15nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, argon is worked gas, sputtering pressure 3.0*10-1Pa, uses witch culture
Vanadium metal is target (witch culture amount: percentage by weight 2.5%), the thicknesses of layers 60nm of deposition.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 15%, sputtering pressure 3.5*10-1Pa reactive sputtering
Deposit high refractive index film/silicon dioxide film composite film, thicknesses of layers 125nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and witch culture vanadium film layer is heat-treated oxidation
Become vanadium dioxide, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 60%；Glass ambient temperature from
42 DEG C of beginnings, coated glass is to 2500nm wavelength infrared reflection rate 55%；Film hardness 6.5H；Coated glass stands 1000
Secondary 300 DEG C～the thermal shock in 3.5 hours of 500 DEG C of heat radiations.
Embodiment 5
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 25%, sputtering pressure 3.5*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 13nm of deposition.
2, it is coated with infrared-reflecting layers: in vacuum chamber, oxygen and argon flow amount ratio 1%, sputtering pressure 3.5*10-1Pa,
It is target, the barium oxide thicknesses of layers 60nm of deposition anoxia with vanadium metal.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 25%, sputtering pressure 3.5*10-1Pa reactive sputtering
Deposit high refractive index/silica composite films, thicknesses of layers 100nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and vanadium film layer is heat-treated and is oxidized to dioxy
Change vanadium, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 65%；Glass ambient temperature from
62 DEG C of beginnings, coated glass is to 2500nm wavelength infrared reflection rate 55%；Film hardness 5.5～6.5H；Coated glass 1000
Secondary standing 350 DEG C～500 DEG C of heat radiations 3.5 hours, coated glass stands 1000 300 DEG C～500 DEG C of little intermittent fever of heat radiation 3.5
Impact.
Embodiment 6
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 20%, sputtering pressure 3.5*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 50nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, oxygen and argon flow amount ratio 1%, argon works gas, sputtering
Air pressure 4.0*10-1Pa, does target (witch culture amount: percentage by weight 3.5%), the vanadium oxide of deposition anoxia with witch culture vanadium metal
Thicknesses of layers 60nm.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 25%, sputtering pressure 3.5*10-1Pa reactive sputtering
Deposit high refractive index/silica composite films, thicknesses of layers 125nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and witch culture vanadium film layer is heat-treated oxidation
Become vanadium dioxide, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 55%；Glass ambient temperature from
32 DEG C of beginnings, coated glass is to 2500nm wavelength infrared reflection rate 65%；Film hardness 6.5H；1000 warps of coated glass
By 350 DEG C～500 DEG C of heat radiations 3.5 hours, coated glass stands 1000 300 DEG C～the thermal shocks in 3.5 hours of 500 DEG C of heat radiations.
Embodiment 7
1, it is coated with sealing coat: in vacuum chamber, oxygen and argon flow amount ratio 20%, sputtering pressure 3.0*10-1Pa, with pure silicon,
Or sial or silicon boron do target, the silicon oxide film layer thickness 15nm of deposition.
2, being coated with infrared-reflecting layers: in vacuum chamber, argon is worked gas, sputtering pressure 4.0*10-1Pa, uses witch culture
Vanadium metal is target (witch culture amount: percentage by weight 3.5%), the thicknesses of layers 50nm of deposition.
3, it is coated with antireflection layer: in vacuum chamber, oxygen and argon flow proportional 20%, sputtering pressure 3.0*10-1Pa reactive sputtering
Deposit high refractive index/silica composite films film, thicknesses of layers 120nm.
4, the coated glass obtained is tempering at atmospheric environment space temperature 600～750 DEG C, and witch culture vanadium film layer is heat-treated oxidation
Become vanadium dioxide, coated glass by tempering.
In 380nm to 1100nm spectral wavelength ranges, the absorbance of this coated glass is 65%；Glass ambient temperature from
35 DEG C of beginnings, coated glass is to 2500nm wavelength infrared reflection rate 60%；Film hardness 6.5H；1000 warps of coated glass
By 350 DEG C～500 DEG C of heat radiations 3.5 hours, coated glass stands 1000 300 DEG C～the thermal shocks in 3.5 hours of 500 DEG C of heat radiations.
Claims (3)
1. the preparation method of a thermic reflection infrared ray coated glass, it is characterised in that comprise the following steps:
1) magnetically controlled sputter method is used to be coated with silicon dioxide sealing coat on high-boron-silicon glass substrate；
2) magnetically controlled sputter method is used to be coated with vanadium metal film layer on sealing coat；With vanadium metal or witch culture vanadium metal as target；
3) use magnetically controlled sputter method to be coated with silicon dioxide film on infrared-reflecting layers and obtain coated glass as antireflection layer；
4) heat treatment at atmospheric environment, space temperature 600～750 DEG C, the oxidation of described vanadium metal film layer forms infrared-reflecting layers,
Coated glass is by tempering simultaneously；
Wherein, described silicon dioxide sealing coat is 10～15nm；Described infrared reflection layer thickness is 20-60nm；Described anti-reflection
Penetrating tunic layer thickness is 70～125nm.
2. thermic reflects the preparation method of infrared ray coated glass as claimed in claim 1, it is characterised in that described witch culture vanadium gold
The doping belonged to is 0-3.5wt%.
3. thermic reflects the preparation method of infrared ray coated glass as claimed in claim 1, it is characterised in that the reflection of described thermic is red
Outside line coated glass is used for heat-resisting sight glass.
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| CN101560638B (en) * | 2009-05-27 | 2010-12-01 | 天津大学 | Method for preparing vanadium oxide film by metal oxidation method |
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