CN106150290B - A kind of thermocolour intelligent dimming energy-saving glass and preparation method thereof - Google Patents
A kind of thermocolour intelligent dimming energy-saving glass and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of thermocolour intelligent dimming energy-saving glass, a kind of thermocolour intelligent dimming energy-saving glass, it is characterised in that it includes the first glassy layer, framework, the glass composite that are bonded successively, the first glassy layer bonds to form hollow glass structure by framework and glass composite；The glass composite is selected from single-glass or laminated glass structure；Glass composite includes the thermocolour intelligence film layer with phase transition function.The present invention realizes heat regulation with variation of ambient temperature, can be widely used in building energy conservation door and window and car and boat door and window fields.Its structure can increase the security performances such as the impact resistance of glass, extend the service life of vanadium oxide composite film, and the secondly selection of a variety of substrate materials can meet the needs of varying environment strength of glass.
Description
Technical field
, can be with the present invention relates to a kind of energy-saving glass that heat regulation is realized with variation of ambient temperature and preparation method thereof
It is widely used in building energy conservation door and window and car and boat door and window fields.
Background technology：
Double glazing is made up of two layers or multi-layer planar glass.The high-strength high-air-tightness compound binding agent of surrounding, by two
Piece or divided glass pass through the sealed glue sticking of framework, sealing.Centre is filled with dry gas, and inframe is filled with drier, to ensure
The aridity of air between sheet glass.It is a kind of good heat-insulated, sound insulation, building beautiful and applicable and that building deadweight can be reduced
Material.It is mainly used in needing heating, air-conditioning, prevent noise or condensation and needing the building without direct sunlight and special light
On.Being widely used in house, restaurant, hotel, office building, school, hospital, shop etc. needs the occasion of room conditioning.Also can use
In train, automobile, steamer, reach in freezer door and window etc..
The usual structure of laminated glass is mainly used in building door to accompany resin film between two unorganic glass plates
Window, car and boat door and window.Laminated glass is compared with common monolithic glass plate, and its impact resistance is more superior, and glass breakage is not easy
Cause personal injury.Therefore laminated glass uses as the glass pane for requiring the sense of security or security.With reference to various resin films,
Laminated glass can realize the superior function for reducing noise, lifting effect of heat insulation of glass composite.Should in high-end glass door and window
With field, not only require that glass has good impact resistance, it is also necessary to which glass has good heat preservation and insulation, therefore
It is highly desirable that the glass product of hollow structure will be synthesized on the basis of laminated glass, its sound insulation and effect of heat insulation are further
Embody.
Vanadium oxide is a kind of transition metal oxide with phase-change characteristic.Vanadium oxide monocrystal material can occur at 68 DEG C
Phase in version, the quadratic metal state being changed into from the monocline semiconductor form of low temperature under high temperature, that is, it is (high to R phases that M phases (low-temperature phase) occur
Warm phase) transformation.While phase structure changes, the optics of vanadium oxide material, electricity, the physical property such as magnetics also dashes forward
Become.In optics aspect, vanadium oxide can be by the infrared transparent state of low temperature to the infrared external reflection state of high temperature due to the transformation of structure
Transformation, it is final to realize the solar energy carried out as temperature environment changes so as to reach the purpose of reflection infrared ray and sunshine
Regulation.The phase transition temperature of vanadium oxide can be adjusted by the content of dopant, from 25 DEG C to 68 DEG C.Therefore, oxygen is used
The purpose of Intelligent adjustment sunshine and infrared ray can be realized by changing film prepared by vanadium, in energy-saving coating, optical memory material, laser
Protection etc. has extensive purposes.
The currently used method for preparing vanadium oxide film mainly has magnetron sputtering method, chemical vapour deposition technique, colloidal sol to coagulate
Glue method etc..Can be divided into terms of the technological process of preparation after the disposable deposition film of high temperature and low temperature or normal temperature deposition carry out it is quick
Heat-treatment of annealing, including directly prepared on a glass substrate by chemical spray method, by magnetron sputtering method in high temp glass base
Short annealing is carried out on body under the thermals source such as radiation fluorescent tube after Magnetron Sputtering Thin Film under deposition film and normal temperature to be had
There is the film of phase transition function.Preparation temperature based on the requirement of vanadium oxide film crystallization temperature environment, especially large area batch production
400 DEG C~600 DEG C of scope is spent, patent document CN102285766A is using high temeperature chemistry spraying, patent document CN104099563A
Using direct sputter-deposited thin films under hot environment, have in terms of its production efficiency and substrate heatproof or security performance many
Defect, show that the heat resistance that its glass substrate is prepared in above-mentioned temperature environment is affected, glass breakage occur or should
The obvious loss of power, or the efficiency of deposition film are very low.Another aspect patent document CN104060236A and application
Number can preferably be solved for the mode of short annealing after the 201410856240.1 normal temperature deposition film that provides of patent document
The problem of glass breakage and stress are lost.
Still further aspect, related research show that the soaking time of vanadium oxide thermocolour intelligence film layer annealing is longer, then its light
Thermal property is better.For infra-red radiation annealing process route, the film layer factor related to annealing time length, it is film
The thickness and transmitance of layer.It is generally thick in film layer in order to obtain the vanadium oxide thermocolour intelligence film layer of more high visible light transmissivity
Need more accurate in terms of degree and tend to be thinner, the more thin then transmitance of film layer is also of a relatively high.But the thin then equal bar of film layer
The time annealed under part can extend, and cause film layer to reduce effective absorptivity of radiation ray, film layer is thinner to reach moving back for crystallization
Fiery temperature-time is longer.The glass basis heated time is longer in this process, and the total amount of heat of absorption is more, especially for
It is easier the problem of tempering stress loss occur for safety glass substrate, this is done in patent document CN104060236A
Detailed analytic explanation.Research process also found that ordinary plate glass glass breakage occurs before and after being annealed using infra-red radiation
Probability it is smaller, and the long period heating will not produce so-called stress degenerate problem.For chemically toughened glass substrate
Speech, the reason for Crack cause of stress is formed from physical toughened glass surface stress, are different, and it is moved back infra-red radiation fluorescent tube
It is also not in the loss of the tempering stress of short time in fire environment.Therefore can be in ordinary glass substrate or chemical tempering
The vanadium oxide thermochromatic coating of deposited amorphous state on glass substrate, then obtained using infra-red radiation annealing way with higher visible
The thermochromatic coating of the phase transition function of light transmission rate.
The content of the invention
The application demand of the technical problem run into and correlation, this hair are prepared based on vanadium oxide thermocolour intelligent glass complex
It is bright to adopt the technical scheme that by vanadium oxide composite film (thermocolour intelligence film layer) structure reasonable in design, in a variety of glass bases
Deposited amorphous state vanadium oxide film layer and its protective layer on piece, glued after short annealing is handled with another glass substrate by framework
Knot forms hollow glass structure complex, obtains thermocolour intelligent dimming energy-saving glass.Such glass composite can increase glass
The security performances such as the impact resistance of glass, extend the service life of vanadium oxide composite film, secondly the selection of a variety of substrate materials can be with
Meets the needs of varying environment strength of glass.
To achieve these goals, the present invention uses following technical scheme：
A kind of thermocolour intelligent dimming energy-saving glass, including the first glassy layer, framework, the glass composite being bonded successively, the
One glassy layer bonds to form hollow glass structure by framework and glass composite；The glass composite be selected from single-glass or
Laminated glass structure；
When glass composite is single-glass, there is phase towards the first glassy layer side surface attachment in the single-glass
Become the thermocolour intelligence film layer of function；
When glass composite is laminated glass structure, glass composite includes the second glassy layer, the film being bonded successively
With the 3rd glassy layer, the second glassy layer and the 3rd glassy layer bond to form glass composite by film；Wherein, in the second glass
Aspect is to the side surface of film one or the second glassy layer towards a side surface of the first glassy layer or the 3rd glassy layer towards film
Side surface attachment there is the thermocolour intelligence film layer of phase transition function；When forming hollow glass structure, the second glassy layer is located at face
To the side of the first glassy layer；
Above-mentioned thermocolour intelligence film layer includes vanadium oxide film layer and is arranged at the protective layer of the vanadium oxide film layer both sides.
Hollow glass structure in the present invention, which refers to be isolated between glass composite and the first glassy layer by framework, to be formed
Sealing cavity structure, refer to double glazing of the prior art.Similar with the double glazing of routine, the framework can
To be frame-generic or be filled with the framework of molecular sieve, the conventional molecular sieve of double glazing product can be applied to this
Invention.Molecular sieve can adsorb moisture and residual organic matter in double glazing simultaneously, make double glazing even in very low temperature
Under remain in that clear transparent, while can fully reduce double glazing because the great variety in season and day and night temperature born it is strong
Big external and internal pressure is poor, extends the service life of double glazing.Frame thickness can be 6mm~30mm, and hollow intracavitary can be filled with
N2 or inert gas, wherein inert gas Ar are the gas choosings for preparing the high performance-price ratio with more preferable thermal property energy-saving glass
Select.
The phase transition function refers to that the vanadium oxide in thermocolour intelligence film layer, present invention is more particularly directed towards V：O atom ratio close to
1：2 vanadium dioxide thermo smart membrane.Phase in version occurs in a certain specified temp, infrared ray is presented under low temperature and sunshine passes through
Characteristic, infrared ray and sun reflective character are presented under high temperature.
Single-glass of the present invention (is illustrated and distinguished with the glassy layer in laminated glass, hereinafter referred to as convenience
4th glassy layer), and first, second, and third glassy layer is plate glass, species is not particularly limited.I.e., it is possible to use sodium
Lime glass, lead glass, alkali-free glass, quartz glass, alumina silicate glass, pyrex, phosphate glass, tellurides glass
The various glass materials such as glass, titanate glass, fluoride glass, Lithium silicate glass.Each glassy layer used in the present invention can
Think identical material, can also different materials.The thickness of used plate glass can be different, and glass self-strength can not
Together, you can to select general glass to lead to (non-stressed reinforcing glass), semi-tempered glass or safety glass.The toughening method of safety glass
It can be physical toughened or chemically toughened glass.Thickness can select 3mm~10mm, more preferably 4mm~6mm.
For whether using stress enhancing safety glass, first, second, third glassy layer and list of the present invention
Simple glass, semi-tempered glass or safety glass can be respectively adopted in layer glass.Such as, it is laminated glass knot for glass composite
Structure, following structure can be used.
1) the first glassy layer is safety glass, and second, third glassy layer is non-safety glass,；
2) the first glassy layer is safety glass, and the second glassy layer is non-safety glass, and the 3rd glassy layer is safety glass；
3) first, second and third glassy layer is safety glass；
4) 1) can be semi-tempered glass to the safety glass in 3) structure.
Secondly for thermocolour intelligence film layer position, when glass composite is single-glass, it is preferably placed at face
To middle cavity (i.e. towards the first glassy layer) side；When glass composite is laminated glass structure, can select：
1) it is located at the second glassy layer towards the side of middle cavity (i.e. towards the first glassy layer)；
2) it is located at the second glassy layer towards the side of film；
3) it is located at the 3rd glassy layer towards the side of film；
Above-mentioned material and the thermocolour intelligent dimming energy-saving glass of structure type can prepare, comprehensive safety factor
Consideration, the 3rd glassy layer, the 4th glassy layer are typically chosen safety glass or semi-tempered glass, prioritizing selection safety glass base
Piece, said structure glass can select the glass of 4~10mm thickness, and specific thickness selection will illustrate in conjunction with the embodiments.
It is heretofore described it is physical toughened typically represent in case of no particular description its surface stress intensity for 90MPa~
130MPa safety glass, i.e., complete safety glass；So-called semi-tempered glass refers to that acierage stress is answered between commonly non-
A kind of surface stress reinforcing glass between power reinforcing glass and safety glass, its surface stress is typically in 48Mpa or so.
The preparation method of safety glass is broadly divided into physical toughened method and chemical tempering process, it is conventional it is physical toughened be by glass
Glass substrate is heated to wind chilling after soft state so that glass has 90MPa~130MPa stress intensity, if certainly using
Then glass has 48MPa or so stress intensity to half tempered mode.Chemical tempering process generally use low-temperature ion exchange process will be molten
Such as Na in big ion exchange glass material in salting liquid+, 450Mpa or so surface stress can be formed.
Heretofore described thermocolour intelligence film layer refers to comprising the composite film including vanadium oxide film layer, can be two layers
The film layer of film, trilamellar membrane and its above.In view of the film layer structure of two membranes reality production and weather-proof failure in terms of not
With obvious advantage, therefore the composite film of three layers and its above is typically chosen, especially the both sides of vanadium oxide film layer, which are set, protects
Sheath, film layer structure main purpose as design is to protect vanadium oxide film layer, if vanadium oxide film layer is directly and glass surface
Then there is in film layer preparation process and its in the follow-up long period Na inside glass in contact+Intrusion etc. harmful components causes oxygen
Change the hydraulic performance decline of vanadium functional film layer.Based on similar consideration, when vanadium oxide thermocolour intelligence film layer and film contact
Need to set protective layer between vanadium oxide film layer and film, avoid the organic matter in film from invading functional film layer.Described guarantor
Cuticular layer can select metallic diaphragm, metal oxide, metal nitride, metal oxynitride etc., such as NiCrOx, as long as can
Keep certain time internal resistance every the intrusion of harmful substance and itself do not produce the material of the negative effect to vanadium oxide film performance
Material can use.In multi-layer film structure the effect of other media coatings be light thermal property, physicochemical property (such as wearability) with
And the regulation and control in terms of color.
Preferably, above-mentioned thermocolour intelligence film layer includes first medium layer, vanadium oxide film layer, the second medium set gradually
Layer.
Further, it is also provided with infrared external reflection between vanadium oxide film layer and first medium layer or/and second medium
Layer.
Further, the first barrier layer and the second resistance can also be disposed between vanadium oxide film layer and second dielectric layer
Barrier.
Further, the first barrier layer is also provided between vanadium oxide film layer and first medium layer.
Further, heretofore described thermocolour intelligence film layer can also select following common structure, but not
Restriction as the functional film layer structure.Wherein, glass refers to the glassy layer for being coated with thermocolour intelligence film layer.
1) barrier layer of glass/first barrier layer/vanadium oxide film layer/first；
2) glass/first medium layer/infrared reflecting layer/vanadium oxide film layer/second dielectric layer；
3) glass/first medium layer/infrared reflecting layer/vanadium oxide film layer/first barrier layer/second dielectric layer；
4) barrier layer of glass/first medium layer/infrared reflecting layer/first barrier layer/vanadium oxide film layer/first/second is situated between
Matter layer；
5) resistance of the barrier layer of glass/first medium layer/infrared reflecting layer/first barrier layer/vanadium oxide film layer/first/second
Barrier/second dielectric layer；
6) resistance of the barrier layer of glass/first medium layer/infrared reflecting layer/second/the first barrier layer/vanadium oxide film layer/first
Barrier/the second barrier layer/second dielectric layer；
7) barrier layer of glass/first medium layer/second barrier layer/infrared reflecting layer/second/the first barrier layer/vanadium oxide
The barrier layer of film layer/first/the second barrier layer/second dielectric layer；
8) glass/first medium layer/vanadium oxide film layer/first barrier layer/second dielectric layer；
9) glass/first medium layer/first barrier layer/vanadium oxide film layer/first barrier layer/second dielectric layer；
10) barrier layer/second of the barrier layer of glass/first medium layer/first barrier layer/vanadium oxide film layer/first/second is situated between
Matter layer；
11) resistance of the barrier layer of the barrier layer of glass/first medium layer/second/the first barrier layer/vanadium oxide film layer/first/second
Barrier/second dielectric layer；
12) glass/first medium layer/vanadium oxide film layer/second dielectric layer/first medium layer/vanadium oxide film layer/second is situated between
Matter layer；
13) glass/first medium layer/first barrier layer/vanadium oxide film layer/first barrier layer/second dielectric layer/first is situated between
Matter layer/the first barrier layer/vanadium oxide film layer/first barrier layer/second dielectric layer.
Infrared reflecting layer is metal level (thickness is preferably 5nm~15nm) in said structure, in Pt, Au, Ag, Cu extremely
A kind of few metal or its alloy.The metal material principally falls into precious metal material, wherein the material by taking Au, Ag, Cu as an example exists
It is used as infrared reflective material in LOW-E building energy conservation glass.Infrared reflecting layer can also be with the transparent of infrared external reflection effect
Conductive film layer (thickness is preferably 10nm~150nm), material in ITO, ATO, AZO, FTO or other same type of material at least
It is a kind of.On above-mentioned metal infrared external reflection film layer and compound of red external reflectance film layer, person skilled in art is to hold very much
It is readily understood and acquisition.
First barrier layer is selected from least one of NiCr, Ni, Cr, Ti, Ni alloy, Cr alloys metal corresponding to metal and aoxidized
Thing film, metal nitride films or metal oxynitride film, it can keep more preferable connection effect with vanadium oxide film layer.It is preferred that
Ground, thickness are 1nm~15nm.
Second barrier layer is selected from least one of NiCr, Ni, Cr, Ti, Ni alloy, Cr alloys material, and it can be with first
Barrier layer coordinates the intrusion for playing preferably barrier harmful environmental element, ensures the photo-thermal of vanadium oxide functional film layer long stable effect
Performance.Preferably, thickness is 1nm~15nm.
Vanadium oxide film layer is VOx, wherein 1.75≤x≤2.15, x are average atom number.Preferably, thickness be 30nm~
150nm.The phase transition temperature of pure VOx film layers is 68 DEG C, can be with order to meet the needs of the different phase transition temperatures near the temperature
By adding dopant in VOx film layers, the metal ion of large radius is such as adulterated, thermocolour intelligence can be reduced if W, Mo ion
The phase transition temperature of film layer；Same doping F ion can also reduce the phase transition temperature of thermocolour intelligence film layer；In addition under particular case
The metal ion of minor radius can be adulterated, can raise thermocolour smart membrane side phase transition temperature if Ti, Mg ion, at the same for
Thermocolour intelligence film layer also has some improvement through the yellow phenomenon of colour cast.Therefore, the doped chemical be selected from W, Mo, Nb,
Zn, Mg, F and other materials that can change thermocolour intelligence Phase transition temperature, doping molar percentage are 0.5%~10%,
Material on that can change thermocolour intelligence film layer phase transition temperature contrasts person skilled in art and is readily available very much.For
It is suitable to routine use, the phase transition temperature of the vanadium oxide film layer in the present invention in thermocolour intelligence film layer is preferably adjusted to be less than 55
℃.Further, it is preferable to for less than 35 DEG C., can in order to obtain the phase transition temperature having closer near room temperature in the present invention
By injecting dopant to vanadium oxide film layer, such as to adulterate the metal ion of large radius and nonmetallic F ion, such as to VOx
The tungsten that film layer doping molar concentration is 0.8%, its phase transition temperature are 48.7 DEG C.In order to further obtain more low transformation temperature
VOx film layers, the present invention in VOx film layers always adulterate molar concentration be 1.35% tungsten, its phase transition temperature be 34.2 DEG C.Other root
Show according to current research, the non-other elements that introduce can also obtain the VOx film layers with compared with low transformation temperature, and main cause exists
Cause in the change of VOx membranous layer ingredients, the especially relative oxygen atom that lacks of film layer can then obtain lower phase transition temperature, that is, pass through
Auto-dope mode in preparation process can also change the phase transition temperature of VOx film layers.
Dielectric layer (including first medium layer and second dielectric layer) is oxide, nitride or nitrogen oxides, selected from TiOx
(wherein x=1.7~2.7, preferably x=2~2.6), SixNy (wherein x/y=0.75；Or x/y=0.76~2.3, rich in Si
Situation), SiOx (wherein x=1.7~2.3, preferably 2.0), Nb2O5、ZrO2、SnO2、ZnO2, ZrNx, SixNyOy or
ZnSnO2At least one of, it is preferable that thickness is 30~150nm.The master that above-mentioned first medium layer and second dielectric layer are set
The regulation being to carry out in terms of final composite film appearance color and overall transmitance of syllabus.Its application and current LOW-E
Media coating in energy-saving film is closely similar, as selection of the person skilled in art for above-mentioned dielectric layer material also right and wrong
Often readily.Need to carry out the annealing under hot conditions, above-mentioned deielectric-coating based on the thermocolour smart membrane with phase transition function is obtained
SixNy has excellent resistance to elevated temperatures and crocking resistance, therefore preferred thermocolour smart membrane most table in the present invention in layer material
Layer and be SixNy with the bottom of substrate contact.With glass side (i.e. between vanadium oxide film layer and glass) and composite membrane is most
Surface is protected using SixNy film layers, contributes to the increase of composite film heat resistance, naturally it is also possible to resistance to using ZrNx etc.
The good film material of mill property.
Enumerating for the above-mentioned film layer structure about thermocolour intelligence film layer is not used as its specific limitation, merely to more
Good understands its relevant film layer structure.In implementation process, the film layer of same names can use different material and thickness,
For example being provided with the first barrier layer in the both sides of vanadium oxide film layer, then its thickness can be with different, and material can also respectively not
It is identical.
Further, the thermocolour intelligence film layer is repeatable is superimposed more than one.I.e., it is possible to repeat to apply on a glass substrate
The thermocolour intelligence film layer of a certain structure of cloth., can be with by taking first medium layer/vanadium oxide film layer/second dielectric layer this structure as an example
Repetition is coated with more than one structure, forms such as the first glassy layer/first medium layer/vanadium oxide film layer/second dielectric layer/the
Structure as the glassy layer of one dielectric layer/vanadium oxide film layer/second dielectric layer/film/second；Other knots can also be coated
Structure, first medium layer/infrared reflecting layer/vanadium oxide film layer/second dielectric layer this structure is such as being coated thereon, form such as the
One glassy layer/first medium layer/vanadium oxide film layer/second dielectric layer/first medium layer/infrared reflecting layer/vanadium oxide film layer/the
Structure as the glassy layer of second medium layer/film/second.When in film layer first medium layer and second dielectric layer be chosen for equally into
Second dielectric layer then adjacent in repeat unit can merge into a kind of film layer of composition with first medium layer during the film layer divided, then
Equivalent to a tunic layer.
When glass composite is laminated glass, on its used film, as long as effectively act on glassy layer
Between bonding, obtain desired optical property, there is corresponding thermoplastic property at certain temperature or pressure condition,
Laminated glass complex has sufficiently high visible light transmissivity after making shaping.Such as：Polyvinyl butyral resin (PVB),
EVAc (EVA), polyvinyl alcohol (PVAL), polyethylene (PE), polypropylene (PP), polystyrene (PS),
Polyurethane (PU) etc., wherein film highly developed in terms of applied to building doors and windows or glass of vehicle and ship door and window, can be easy
Improve and the caking property of plate glass, preferably polyvinyl butyral resin (PVB).Heretofore described adhesive sheet generally selects
With 0.3mm~2.28mm PVB or PU materials, the embodiment in the present invention uses transparent PVB materials.Except of course that selection is saturating
Bright PVB materials and other colored PVB materials can also be selected outside.The PVB thickness declared according to the commercialization of PVB industries, can
To carry out the selection of multiple thickness such as 0.38mm, 0.76mm, 1.14mm, 1.52mm, 2.28mm, reaching security performance requirement
Manufacturing cost simultaneously, generally selects binding material of 0.38mm, 0.76mm the PVB films as laminated glass articles.
Especially in the environment of relative confused noise, in order to obtain more quiet comfortable indoor environment, described film can
To select the PVB materials with sound insulation function.As Japanese ponding company produce 0.76mm S-LEC-SAF sound deadening sheets, to room
Outer 80 decibels of sound, compared to the common PVB of same thickness, sound deadening sheet can reduce the sound no less than 5 decibels.
The present invention also provides the preparation method of above-mentioned thermocolour intelligent dimming energy-saving glass.
When glass composite is single-glass, comprise the following steps：(1) according to the structure of thermocolour intelligence film layer, in list
Layer glass surface is sequentially depositing layers of material, obtains film-coated glass substrate；It is (heavy that the thermocolour intelligence film layer includes vanadium oxide film layer
Belong to amorphous vanadium oxides during product, be changed into crystalline state after annealing, so as to having above-mentioned phase transition function) and it is arranged at the vanadium oxide
The protective layer of film layer both sides, plated film are carried out by the way of sputtering or coating；(2) film-coated glass substrate is made annealing treatment,
Obtain glass composite；(3) the first glassy layer, framework, glass composite (are adhered into the 4th glass of thermocolour smart membrane layer
Layer) overlap successively, hollow glass structure is formed using sealing gluing knot, obtains the thermocolour intelligent dimming energy-saving glass；Wherein,
The side of glass composite attachment thermocolour smart membrane layer is towards the first glassy layer；
When glass composite is laminated glass structure, comprise the following steps：(1) according to the structure of thermocolour intelligence film layer,
In the second glassy layer towards the side surface of film one or the second glassy layer towards a side surface of the first glassy layer or the 3rd glass
Aspect is sequentially depositing layers of material to a side surface of film, obtains film-coated glass substrate；The thermocolour intelligence film layer includes oxygen
Change vanadium film layer (belong to amorphous vanadium oxides during deposition, be changed into crystalline state after annealing, so as to have above-mentioned phase transition function) and set
The protective layer of the vanadium oxide film layer both sides is placed in, plated film is carried out by the way of sputtering or coating；(2) film-coated glass substrate is entered
Row annealing；(3) the second glassy layer, film, the 3rd glassy layer are stacked successively, by suppressing (such as hot-forming) formation glass
Glass complex；(4) the first glassy layer, framework, glass composite are overlapped successively, double glazing knot is formed using sealing gluing knot
Structure, obtain the thermocolour intelligent dimming energy-saving glass；Wherein, the second glassy layer is located at towards the first glassy layer in glass composite
Side.
Above-mentioned plating steps can specifically use procedure below：Plated film is carried out under normal temperature or low temperature to glass substrate, is plated
Film is carried out by the way of sputtering or coating；Ready glass substrate, which enters under vacuum environment, carries out plated film, and the present invention can be with
Deposition plating is carried out using the methods of such as magnetron sputtering, electron beam evaporation, ion beam sputtering, laser splash, with more business
Change application and reach batch production advantage for magnetically controlled sputter method, therefore it is preferred that magnetron sputtering.Designed according to film layer structure, glass
Vanadium oxide film layer and each protective layer are sequentially depositing on substrate, such as, when composition hinders for the first glassy layer/first medium layer/first
During barrier/infrared reflecting layer/vanadium oxide film layer/first barrier layer/second dielectric layer/film/second glassy layer, successively with first
Dielectric layer target, the first barrier layer target, infrared external reflection film layer target, vanadium oxide film layer target, the second barrier layer target and
Second dielectric layer target as sputter plated film, ultimately form composite film (the i.e. vanadium oxide thermocolour intelligence of amorphous vanadium oxide film layer
Film layer).
Above-mentioned that film-coated glass substrate is made annealing treatment, acquisition has the step of thermocolour intelligence film layer of phase transition function
In, the preferred radiant type heating of annealing way；According to different film layer structures, its environment annealed and atmosphere requirements are not
Together, you can to select annealing under vacuum environment atmosphere to select to anneal under atmospheric environment.With reference to its annealing of the production of reality
For temperature range at 400 DEG C~700 DEG C, annealing time is tens of seconds not wait (such as 40s~420s) to several minutes.Vacuum environment atmosphere
It is lower annealing be annealing vacuum cavity vacuumize the base vacuum for reaching predetermined after, toward vacuum cavity in be filled with inertia, oxidisability,
Reducing atmosphere, N may be selected2、Ar、O2、H2Etc. atmosphere.According to different vanadium oxide thermocolour intelligence membranous layer ingredients and film layer knot
The annealing atmosphere composition of structure selection is different.
If the film-coated glass substrate of selection is non-tempering stress reinforcing glass substrate in preparation method step, then remaining is such as
The safety glass substrate in need for providing stress enhancing, can be used ready-made safety glass, or the preparation process the step of
(1) tempering processing, is carried out before or after (2).
When glass composite is laminated glass structure, its preparation method mainly has two kinds, the method that one uses roll-in,
Secondly laminated glass is prepared using vacuum pumping method.
Such as roll-in method：Coated glass, film are stacked successively, without coated glass, the semi-finished product laminated glass combined, pass through
Heating, roll-in are allowed to be molded.Rolling pressure is 3bar~6bar, and glass surface temperature reaches 40~75 DEG C after heated roll-in.
Then glass is sent into autoclave and carries out HTHP shaping, the pressure of autoclave is 1MPa~1.6MPa, autoclave temp
Scope is 100 DEG C~160 DEG C.Such as, rolling pressure can be set as 5bar, about 65 DEG C of surface temperature, the pressure of autoclave is
1.4MPa, the temperature of autoclave is 145 DEG C.Thermocolour intelligence film layer in the present invention can be arranged in glass composite (i.e. with
Film is adjacent), can also be arranged on the outside of glass composite (when being arranged on the outside of glass composite, be preferably disposed on towards
The side of middle cavity).
Such as vacuumizing method：Coated glass, film are stacked successively, without coated glass, the semi-finished product laminated glass combined, put
Enter in the vacuum bag that can keep vacuum tightness environment, be finally put into autoclave, its vacuum bag have bleeding point with the external world it is true
Empty pump group is wanted to connect, and autoclave vacuum bag during increasing temperature and pressure keeps the lasting state vacuumized, after HTHP
Interlayer composite glass body is formed, the pressure of its autoclave is 1MPa~1.6MPa, and autoclave temp scope is 100 DEG C~160 DEG C.
Such as, rolling pressure can be set as 5bar, about 65 DEG C of surface temperature, the pressure of autoclave is 1.4MPa, and the temperature of autoclave is 145
℃.Thermocolour intelligence film layer in the present invention can be arranged in glass composite (i.e. adjacent with film), can also be arranged at glass
On the outside of glass complex (when being arranged on the outside of glass composite, thermocolour intelligence film layer should be arranged at towards the side of middle cavity).
Above-mentioned thermocolour intelligent dimming energy-saving glass and preparation method thereof has following advantage：
(1) the suitable vanadium oxide composite film (thermocolour intelligence film layer) of design is encapsulated in inside glass composite, is had
There is delaying aging to increase service life；Moreover, vanadium oxide film layer is not directly contacted with glass and film, avoid because of adjacent materials
Caused by composition intrusion the problems such as hydraulic performance decline；
(2) there is more preferable energy-saving effect for the laminated glass of other attachment LOW-E film layers, especially infrared
Region has with the characteristic of environment temperature light regulating；
(3) simple glass of non-tempering stress enhancing can be chosen in terms of the selection of vanadium oxide film-coated glass substrate and is answered
The safety glass of power enhancing meets different use demands, and chemically toughened glass substrate can be used under particular case as energy-conservation glass
Raw material prepared by glass obtain more preferable impact strength.
(4), can be appropriate in terms of annealing time in order to obtain the light thermal property required for more high visible light transmissivity etc.
Extend, because this layer of glass is packaged in the inside of hollow structural glass, and bonded by film, therefore the peace such as tempering stress loss
The problem of full aspect of performance, is readily solved.
Brief description of the drawings
Fig. 1：The thermocolour intelligent dimming energy-saving glass structural representation of embodiment 1；
Fig. 2：The thermocolour intelligent dimming energy-saving glass structural representation of embodiment 10；
In figure：1. the framework of molecular sieve is filled with the first glassy layer, 2., 3. fluid sealants, cavity in 4., 5. second glass
Layer, 6. films, 7. thermocolour intelligence film layers, 8. the 3rd glassy layers, 9. the 4th glassy layers.Wherein, the three, the 4th glassy layer faced chamber
Outer side.
Embodiment
Embodiment 1
With reference to described in Fig. 1, the energy-saving glass structure of the embodiment is followed successively by：First glassy layer (the physical toughened glass of 10mm
Substrate), the framework (and fluid sealant), the second glassy layer (the physical toughened glass substrates of 4mm), the film that are filled with molecular sieve
(the transparent PVB of 0.76mm), thermocolour intelligence film layer (being located at the 3rd glassy layer towards the side of film), the 3rd glassy layer (4mm physics
Safety glass substrate).
Preparation method is as follows：
(1) glass substrate is provided.The common float glasses of 2 4mm are carried out physical toughened formation surface stress 100MPa's
Glass substrate (being respectively the second glassy layer and the 3rd glassy layer), the common float glasses of 1 10mm carry out physical toughened formation table
Face stress 100MPa glass substrate (the first glassy layer).
(2) depositional coating.Using vacuum magnetic-control sputtering method in normal temperature environment in the 3rd glass layer by multiple
Different target material depositions form G/SixNy (30nm)/VOx (120nm)/SixNy (150nm), and (G represents the attaching of thermocolour intelligence film layer
Film layer structure glassy layer, similarly hereinafter).X=2 in wherein VOx, x are average atom number, can pass through XPS (x-ray photoelectron energy
Spectrum) carry out test acquisition.
(3) film layer is annealed.The 3rd glassy layer after plated film is carried out using infrared radiation heating in vacuum atmosphere environment
Annealing；The power density of infrared light supply is 120KW/m2, annealing time 58s；
(4) prepared by glass composite.Glass substrate (the 3rd glassy layer) film surface after annealing is placed, stacked successively upwards
0.76mmPVB, the second glassy layer, HTHP is carried out by being put into autoclave after rolling methods precompressed and is molded that to form glass compound
Body.
(5) hollow glass structure is prepared.By glass composite, it is filled with the framework and the first glassy layer layer successively of molecular sieve
It is folded, by sealing gluing knot, final hollow glass structure is formed, wherein the second glassy layer is adjacent with middle cavity.In the step,
If vanadium oxide thermocolour intelligent light modulation film is located at middle cavity side, typically this is needed before hollow glass structure is prepared
Glassy layer edge removes film process.
In production method, if directly using the substrate for having already passed through tempering processing or the base commonly handled without tempering
Piece, then (1) step can omit, i.e., directly using glass substrate carry out plated film.
Frame thickness can be 6mm-30mm, and N2 or inert gas, wherein inert gas Ar can be filled with hollow cavity
It is the gas selection for preparing the high performance-price ratio with more preferable thermal property energy-saving glass, Ar gases is filled with the present embodiment.
Embodiment 2
Compared to embodiment 1, difference is, second, third glassy layer is 4mm semi-tempered glass substrates, the first glass
Glass layer is the physical toughened glass substrates of 5mm, and thermocolour intelligence film layer is deposited on the second glassy layer substrate surface, the film layer structure of deposition
For G/ITO (150nm)/VOx (150nm)/SixNy (50nm).VOx x=2.15, x are average atom number.Annealing time 55s.
Prepare and stack the 3rd glassy layer, 0.76mmPVB, the glassy layer of plated film second during interlayer successively, film surface is positioned at topmost (i.e. most
Thermocolour intelligence film layer cavity side in sealing afterwards).Then it is molded to form glass using vacuumizing mode and carry out HTHP
Complex.
Embodiment 3
Compared to embodiment 1, difference is, second, third glassy layer is common 4mm float glasses, and thermocolour is intelligent
Film deposition in the second glassy layer substrate surface, film layer structure be G/SixNy (80nm)/NiCrOx (1nm)/VOx (30nm)/
NiCrOx(15nm)/SixNy(150nm).X=1.75 in VOx, x are average atom number.Annealing time 135s.Prepare interlayer mistake
The 3rd glassy layer, 0.76mmPVB, the glassy layer of plated film second are stacked in journey successively, film surface is adjacent with PVB films, then using roller
Pressure mode carries out HTHP and shapes to form glass composite, and thermocolour intelligence film layer is located at the second glassy layer towards film side.
Embodiment 4
Be compared to embodiment 1 with part, the 3rd glassy layer be 6mm physical toughened glass substrate, the second glassy layer
For the common float glasses of 4mm, thermocolour intelligence film layer is deposited on the second glassy layer substrate surface, film layer structure G/SixNy
(80nm)/NiCr(1nm)/NiCrOx(1nm)/VOx:W (150nm)/NiCrOx (15nm)/Ni (15nm)/SixNy (150nm),
Wherein VOx:W represents doping W vanadium oxide film layer.X=2 in VOx, x are average atom number, and incorporation molar concentration is 0.8%
Tungsten, annealing time 35s.Prepare and stack the 3rd glassy layer, 0.76mmPVB, the glassy layer of plated film second, film surface successively during interlayer
It is adjacent with PVB films, HTHP is then carried out using roll-in mode and shapes to form outside glass complex.Made in the embodiment
Standby about 48.7 DEG C of its phase transition temperature of vanadium oxide thermocolour smart membrane.
Embodiment 5
For embodiment 4, difference is 6mm semi-tempered glass as the second glassy layer, thermocolour smart membrane
Layer is deposited on the second glassy layer substrate surface, and structure is G/SixNy (30nm)/AZO (10nm)/NiCrOx (4nm)/VOx:W
(80nm)/NiCrOx(15nm)/Ti(1nm)/SixNy(150nm).X=2 in VOx, x are average atom number, mix molar concentration
For 1.5% tungsten, annealing time 50s.Prepare and stack the 3rd glassy layer, 0.76mmPVB, the second glass successively during interlayer
Layer, film surface is adjacent with PVB films, and then carrying out HTHP using roll-in mode shapes to form outside glass complex.The reality
Apply the about 35.6 DEG C of of its phase transition temperature of vanadium oxide thermocolour smart membrane prepared in example
Embodiment 6
For embodiment 4, difference is that the 3rd glassy layer is 4mm chemically toughened glass, thermocolour smart membrane
Layer is deposited on the 3rd glassy layer substrate surface, and film layer structure is G/SixNy (30nm)/NiCr (1nm)/Ag (5nm)/NiCr
(2nm)/NiCrOx (1nm)/VOx (30nm)/NiCrOx (1nm)/NiCr (10nm)/SixNy (70nm), annealing time 65s.The
Two glassy layers are the common float glasses of 4mm, and the first glassy layer is the physical toughened glass of 6mm.The annealing of film layer is in atmospheric environment
Implement, it is not small relative to the common PVB sound transmission loss of same thickness as film, its soundproof effect using 0.76mm sound insulation PVB
In 5 decibels.
Embodiment 7
It is compared to the difference of embodiment 6, forms the superposition of thermocolour intelligence film layer, the film layer of vanadium oxide thermocolour film layer
Structure is G/ZrO2(30nm)/VOx(40nm)/ZrO2(60nm)/ZrO2(30nm)/VOx(40nm)/NiCrOx(3nm)/ZrO2
(60nm), wherein VOx x=2, x are average atom number.Annealing time 70s.
Embodiment 8
Compared to embodiment 3, difference is, the material of two SixNy layers replaces with Nb2O5。
Embodiment 9
Compared to embodiment 3, difference is, the material of two SixNy layers replaces with SnO2。
The thermocolour intelligent dimming glass of above-mentioned similar example 1 to 9 can apply to building energy conservation door glass.
Embodiment 10
With reference to described in Fig. 2, the energy-saving glass structure of the embodiment is followed successively by：First glassy layer (the physical toughened glass bases of 4mm
Piece), the framework (and fluid sealant) that is filled with molecular sieve, thermocolour intelligence film layer is (positioned at the 4th glassy layer towards the first glassy layer
Side), the 4th glassy layer (the physical toughened glass substrates of 4mm)
Preparation method is as follows：
(1) glass substrate is provided.The common float glasses of 2 4mm are carried out physical toughened formation surface stress 100MPa's
Glass substrate (being respectively the first glassy layer and the 4th glassy layer).
(2) depositional coating.Using vacuum magnetic-control sputtering method in normal temperature environment in the 4th glass layer by multiple
Different target material depositions form G/SixNy (30nm)/VOx (80nm)/SixNy (150nm) film layer structure, x=2 in wherein VOx,
X is substantially average atom number.
(3) film layer is annealed.The 4th glassy layer after plated film is carried out using infrared radiation heating in vacuum atmosphere environment
Annealing, annealing time 65s；
(4) hollow glass structure is prepared.Intelligently adjusted above-mentioned by vanadium oxide thermocolour of the annealing with phase transition function
Light film glass layer (the 4th glassy layer), it is filled with the framework of molecular sieve and the first glassy layer stacks gradually, by sealing gluing knot,
Final hollow frame structure is formed, vanadium oxide thermocolour intelligent light modulation film is carried out typically before hollow structure is formed in the step
The edge of glassy layer removes film process.
If it can directly be omitted as raw material, (1) step using safety glass substrate.
Frame thickness can be 6mm-30mm, and N can be filled with hollow cavity2Or inert gas, wherein inert gas Ar
It is the gas selection for preparing the high performance-price ratio with more preferable thermal property energy-saving glass, Ar gases is filled with the present embodiment.
Such a structure thermocolour intelligent dimming glass can be used in vehicle glass door and window and building energy conservation door and window, especially
Frame thickness is smaller, such as thickness is 6mm, can apply to automotive glazing.
In terms of the annealing of embodiment its film plating substrate in the present invention, annealed using infra-red radiation in 30s to 120s times
It is interior to complete crystallization.
The tempering methods of glass substrate, thickness of glass, PVB thickness and film layer in the embodiment to sum up provided
The relevant parameters such as structure selection only as it is a kind of can preferably realize certain structure, reach certain security performance and necessarily
The structural form of the indicator of costs, it is not intended as any restriction of the present invention.
Claims (10)
1. a kind of thermocolour intelligent dimming energy-saving glass, it is characterised in that including the first glassy layer, framework, the glass being bonded successively
Complex, the first glassy layer bond to form hollow glass structure by framework and glass composite；The glass composite is selected from
Single-glass or laminated glass structure；
When glass composite is single-glass, there is phase transformation work(towards the first glassy layer side surface attachment in the single-glass
The thermocolour intelligence film layer of energy；
When glass composite is laminated glass structure, glass composite includes the second glassy layer, the film and the being bonded successively
Three glassy layers, the second glassy layer and the 3rd glassy layer bond to form glass composite by film；Wherein, in the second glass aspect
To the side surface of film one or the second glassy layer towards a side surface of the first glassy layer or the 3rd glassy layer towards the one of film
Thermocolour intelligence film layer of the side surface attachment with phase transition function；When forming hollow glass structure, the second glassy layer is located at towards the
The side of one glassy layer；
The thermocolour intelligence film layer includes vanadium oxide film layer and is arranged at the protective layer of the vanadium oxide film layer both sides.
2. thermocolour intelligent dimming energy-saving glass as claimed in claim 1, it is characterised in that the protective layer is selected from first medium
Layer or second dielectric layer or the first barrier layer or the second barrier layer or infrared reflecting layer or one or more combinations.
3. thermocolour intelligent dimming energy-saving glass as claimed in claim 2, it is characterised in that the thermocolour intelligence film layer include according to
The first medium layer of secondary setting, vanadium oxide film layer, second dielectric layer.
4. thermocolour intelligent dimming energy-saving glass as claimed in claim 3, it is characterised in that in the thermocolour intelligence film layer, oxygen
Change and be additionally provided with infrared reflecting layer between vanadium film layer and first medium layer or/and second medium.
5. thermocolour intelligent dimming energy-saving glass as claimed in claim 3, it is characterised in that in the thermocolour intelligence film layer, oxygen
Change and be disposed with the first barrier layer and the second barrier layer between vanadium film layer and second dielectric layer.
6. thermocolour intelligent dimming energy-saving glass as claimed in claim 5, it is characterised in that in the thermocolour intelligence film layer, oxygen
Change and be additionally provided with the first barrier layer between vanadium film layer and first medium layer.
7. the thermocolour intelligent dimming energy-saving glass as described in claim 2 to 6 is any, it is characterised in that the dielectric layer is selected from
SixNy、SiOx、TiOx、Nb2O5、ZrO2、SnO2、ZnO2, ZrNx, SixNyOz or ZnSnO2At least one of；Described first
Barrier layer is selected from metal oxide film, metal nitride corresponding at least one of NiCr, Ni, Cr, Ti, Ni alloy, Cr alloys
Film or metal oxynitride film；Second barrier layer is selected from least one of NiCr, Ni, Cr, Ti, Ni alloy, Cr alloys material
Material；The infrared reflecting layer is metal level, selected from least one of Pt, Au, Ag, Cu or Al metal or alloy, or for
At least one of transparent conductive film layer of infrared external reflection effect.
8. the thermocolour intelligent dimming energy-saving glass as described in claim 2 to 6 is any, it is characterised in that the thermocolour smart membrane
Layer is repeatable to be superimposed more than one.
9. the thermocolour intelligent dimming energy-saving glass as described in claim 2 to 6 is any, it is characterised in that the vanadium oxide film layer
Phase transition temperature be less than 55 DEG C；The film is the transparent or colored high molecule plastic film with adhesive property, and thickness is
0.3mm~2.28mm；The framework is filled with molecular sieve.
10. the preparation method of thermocolour intelligent dimming energy-saving glass as claimed in claim 1, it is characterised in that
When glass composite is single-glass, comprise the following steps：(1) according to the structure of thermocolour intelligence film layer, in individual layer glass
Glass surface is sequentially depositing layers of material, obtains film-coated glass substrate；(2) film-coated glass substrate is made annealing treatment, obtains glass
Glass complex；(3) the first glassy layer, framework, glass composite are overlapped successively, double glazing knot is formed using sealing gluing knot
Structure, obtain the thermocolour intelligent dimming energy-saving glass；Wherein, the side of glass composite attachment thermocolour smart membrane layer is towards first
Glassy layer；
When glass composite is laminated glass structure, comprise the following steps：(1) according to the structure of thermocolour intelligence film layer,
Two glassy layers are towards the side surface of film one or the second glassy layer towards a side surface of the first glassy layer or the 3rd glass aspect
Layers of material is sequentially depositing to a side surface of film, obtains film-coated glass substrate；(2) film-coated glass substrate is carried out at annealing
Reason；(3) the second glassy layer, film, the 3rd glassy layer are stacked successively, glass composite is formed by compacting；(4) by the first glass
Glass layer, framework, glass composite are overlapped successively, and hollow glass structure is formed using sealing gluing knot, obtain the thermocolour intelligence
Dimming energy-saving glass；Wherein, the second glassy layer is located at towards the side of the first glassy layer in glass composite.
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| TWI613168B (en) * | 2017-01-05 | 2018-02-01 | 國立清華大學 | Smart color window |
| CN107874673A (en) * | 2017-09-29 | 2018-04-06 | 太仓耀华玻璃有限公司 | A kind of laminated glass with electric heating function and preparation method thereof |
| CN108481842A (en) * | 2018-02-11 | 2018-09-04 | 信义玻璃工程（东莞）有限公司 | Large area is floatd side hollow glass and its manufacturing method |
| CN108394352B (en) * | 2018-03-20 | 2019-09-13 | 安徽三联学院 | Car surface protecting film and its spray coating liquor used |
| CN108821604B (en) * | 2018-06-29 | 2021-01-29 | 江苏亿合门窗科技有限公司 | Low-emissivity glass with multifunctional composite characteristics |
| CN109521620A (en) * | 2018-11-01 | 2019-03-26 | 贾英新 | A kind of smart home glass |
| CN109445482A (en) * | 2018-11-08 | 2019-03-08 | 宁波瑞凌节能环保创新与产业研究院 | A kind of composite cooling glass |
| CN110067497A (en) * | 2019-03-12 | 2019-07-30 | 苏州百联节能科技股份有限公司 | A kind of intelligence heat-insulation and heat-preservation anti-theft integrated window |
| CN111061080A (en) * | 2019-12-19 | 2020-04-24 | 南京盈润门窗科技有限公司 | High-transmittance light-changing film plasma inert gas filled combined glass and using method thereof |
| CN111533849B (en) * | 2020-04-23 | 2021-03-19 | 中新国际联合研究院 | Thermotropic type material and intelligent light-adjusting transparent plate of adjusting luminance |
| CN114077081B (en) * | 2021-11-19 | 2023-10-13 | 京东方科技集团股份有限公司 | Dimming glass and preparation method thereof |
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