CN105084776B - A kind of gold solar-control glazing and preparation method thereof - Google Patents
A kind of gold solar-control glazing and preparation method thereof Download PDFInfo
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- CN105084776B CN105084776B CN201410185889.5A CN201410185889A CN105084776B CN 105084776 B CN105084776 B CN 105084776B CN 201410185889 A CN201410185889 A CN 201410185889A CN 105084776 B CN105084776 B CN 105084776B
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Abstract
The invention discloses a kind of golden solar-control glazings and preparation method thereof, and the solar-control glazing includes the glass substrate, stainless steel alloy film, monocrystalline silicon membrane and the metal titanium membrane that closely overlap successively from bottom to top, and the preparation method includes step：1) it is sintered target；2) pretreatment of glass；3) coating film treatment.Coated glass of the present invention in gold, can reach good decorative effect in the sun；Can monolithic use, reduce use cost；Hollow glass is may be made as, reaches preferably control light energy-saving effect.
Description
Technical field
The coated glass prepared the present invention relates to a kind of coated glass preparation method and by this method, more particularly to a kind of sun
The preparation method of photocontrol coated glass and its sunlight controlling coated glass of preparation.
Background technology
Coated glass (Reflective glass) is also referred to as reflecting glass.Coated glass be in one layer of glass surface coating or
Multiple layer metal, alloy or metal compound film to change the optical property of glass, meet certain particular requirement.Coated glass
By the different characteristics of product, following a few classes can be divided into：Heat-reflecting glass, low emissivity glass (Low-E), electropane etc..
There are many production method of coated glass, as vacuum magnetic-control sputtering method, vacuum vapor deposition method, chemical vapour deposition technique and
Sol-gel method etc..Magnetron sputtering film glass can manufacture and design multilayer complexity membrane system using magnetron sputtering technique, can be white
Multiple color is plated out in color glass substrate, the corrosion-resistant and wear-resisting property of film layer is preferable, is current production and most commonly used skill
Art.The kind and quality of vacuum evaporation coating film glass compared with magnetron sputtering film glass there are certain gap, gradually by
Vacuum sputtering replaces.Chemical vapour deposition technique is that reaction gas is passed through on floatation glass production line in scorching hot glass surface
It decomposes, is uniformly deposited on the technology that glass surface forms coated glass.The equipment investment of this method is few, easy-regulating, product into
This is low, chemical stability is good, can hot-working, be one of production method most promising at present.Sol-gel method production plating
Film glass is simple for process, and stability is good, and shortcoming is that product luminous transmittance is too high, decorative poor.
Magnetron sputtering method be application is at most, technique is most stable in current world wide, performance preferably (radiance E values≤
0.12) the coated glass production technology that, kind is most abundant, energy demand is relatively low.Due to this production technology do not need to
Floatation glass production line bundles use, you can float glass and coating film on glass technique separately to be carried out, effectively
Reduce glass post-processing enterprise repeated construction floatation glass production line, reduce CO2 emissions and the relevant energy
Consumption.
The principle of magnetron sputtering plating is to add a quadrature field and electricity between anode in the target pole (cathode) being sputtered
, it is filled with required inert gas (be usually Ar gas) in high vacuum chamber, permanent magnet forms 250 in target surfaces~
The magnetic field of 350 Gausses forms crossed electric and magnetic field with high voltage electric field.Under the action of electric field, argon gas is ionized into cation and electronics,
Added with certain negative high voltage on target, increase from the electronics that target pole is sent out by the effect in magnetic field and the ionization probability of working gas,
Highdensity plasma is formed about in cathode, Ar ions accelerate to fly to target surface under the action of Lorentz force, with very high
Speed bombards target surface, and the atom for being sputtered out on target flies to glass substrate with higher kinetic energy disengaging target surface and deposits film forming.
Application most heat-reflecting glass and low emissivity glass is substantially using vacuum magnetic-control sputtering method and chemical gas at present
Phase sedimentation produces.There is BOC Co. (U.S.) He Laibao in more famous vacuum magnetic-control sputtering method equipment manufacturer in the world
Company (Germany)；There is MB Group Plc (Britain) etc. in Chemical Vapor Deposition Equipment producer.At present, China has occurred hundreds of
There are South China glass group company in coated glass manufacturer of family, the vacuum magnetic-control sputtering method manufacturer being affected in the industry
With Shanghai Sunlight coated glass company etc., there are Shandong blue star glass company and the Changjiang river float glass process glass in chemical vapour deposition technique manufacturer
Glass company etc..
It is numerous to the PRODUCTION TRAITS of golden coated glass at present, such as the patent of invention Shen of Publication No. CN101244898A
A kind of golden low radiation film coating glass please be disclose, glass single face is plated with composite film, and the outermost layer of composite film is one
Protection film layer, composite film include three-layer metal film layer, and wherein layer of metal film layer is copper film layer, and one layer is silver film, is close to
Layer of metal film layer below protection film layer is nichrome film layer or titanium film layer.Its production method includes cleaning, dry and plating
It covers, plating is vacuum magnetic-control sputtering plating, by the target room of dried glass merging vacuum magnetron sputtering coating film equipment successively
Plating composite film.The golden low radiation film coating glass that specific metallic copper, silver make for sputtering target material, color are selected in the invention
Bright-coloured and easy adjusting, stable quality, producing efficiency are high, and still, what this method made is low radiation coated glass (LOW-E glass
Glass), only there is higher reflectivity to far infrared of the wavelength in 4.5-25 micron ranges；Meanwhile Low emissivity made by this method
Glass contains the silver film easily aoxidized, and its oxidation can not only make the color of glass change, and the membrane system can also lost
Low emissivity and heat-insulated performance, therefore it is unable to monolithic use.
Sunlight controlling coated glass prepared by the present invention, overcomes drawbacks described above, to wave-length coverage 350-1800nm's
Sunlight is respectively provided with certain control action, can monolithic use, meanwhile, compared to the silver contained in golden low radiation film coating glass
Layer or layers of copper can make the sunlight controlling coated glass that gold is thin out, prepared by the present invention then there is no the above problem, thus be presented
The more bright-coloured bright eye of gold.
Invention content
The present invention primary and foremost purpose be for above-mentioned existing coated glass technology of preparing there are the problem of a kind of gold is provided
The preparation method of sunlight controlling coated glass and the golden sunlight controlling coated glass of preparation.Gold sun prepared by the method for the present invention
Photocontrol coated glass in gold, can reach good decorative effect in the sun；Visible light transmittance is low, outdoor visible ray is anti-
Penetrate that rate is high, the transmitance of solar energy is low, solar reflectance is high；And the golden solar-control glazing heat transfer coefficient of the present invention
It is low, shading coefficient is low, thermal property is good, effectively thermal energy can be prevented to get in, reduce energy consumption for cooling；Monolithic uses, can
Reach good effect, save use cost；Hollow glass is may be made as, control light energy-saving effect is more preferably.
Purpose to realize the present invention, one aspect of the present invention provide a kind of golden sunlight controlling coated glass, including：
Glass substrate；
First film layer, in glass substrate, first film layer is stainless steel alloy film layer；
Second film layer, in first film layer, second film layer is single crystalline silicon film；
Third membrane layer, in second film layer, the third membrane layer is Titanium film layer.
Wherein, the thickness of first film layer is 9.6-10.4nm, preferably 10nm；The thickness of second film layer is
8.5-8.9nm preferably 8.7nm；The thickness of the third membrane layer is 20-23nm, preferably 21.5nm.
Particularly, there is first film layer, the second film layer, third successively from bottom to top on a surface of glass substrate
Film layer.
Wherein, 50≤L of coated glass film surface reflection colour value*≤ 55,0≤a*≤ 2,24≤b*≤30。
Another aspect of the present invention provides a kind of preparation method of golden sunlight controlling coated glass, is carried out including order below
The step of：
1) it is sintered target
Stainless steel alloy, silicon and titanium are sintered respectively on the target position of the vacuum sputtering room of glass film coating machine, it is spare；
2) pretreatment of glass
The glass of film process to be plated is placed under vacuum state, the glass for treating coating film treatment carries out hydrofuge, degassing process,
The water and gas of glass surface deposition are reduced, hydrofuge, degassing glass is made；
3) coating film treatment
Hydrofuge, degassing glass are sent into the vacuum magnetic-control sputtering room of glass film coating machine, on the surface of hydrofuge, the glass that deaerates
Plating stainless steel alloy film, monocrystalline silicon membrane and titanium film successively from bottom to top.
Wherein, it is >=99.5% that the stainless steel alloy described in step 1), which selects sintering purity, density is >=7.85g/
cm3, fusing point be 1371-1398 DEG C stainless steel (SST) alloy；The silicon select sintering purity be >=99.99%, density be >=
8.57g/cm3；Resistivity is≤0.005-0.20 μ Ω cm；Linear expansion coefficient is：(2~9) × 10-6K-1；Fusing point is 1410 DEG C
Silicon；It is >=99.99% that the titanium, which selects sintering purity, and density is >=4.5g/cm3；Fusing point is 1668 DEG C of titanium.
Particularly, the sintering time of the stainless steel is 30min；The sintering time of the titanium is 30min；The burning of the silicon
The knot time is 200min.
Especially, stainless steel (SST) alloy meets national standard《The stainless steel and refractory steel trade mark and chemical composition
(GB/T20878-2007)》The component requirements of middle 00Cr17Ni12Mo2；The silicon meets national standard《Industrial silicon (GB/
T2881-2008)》The component requirements of middle level-one silicon；The titanium meets national standard《The titanium or titanium alloy trade mark and chemistry into
Divide (GB/T3620.1-2007)》The component requirements of the industrial pure titaniums of TA2 in standard.
Wherein, hydrofuge described in step 2), degassing process are that 2 processing stages of film glass to be plated point are reduced glass surface
The moisture content and gas of deposition, the obtained hydrofuge, degassing glass, wherein the absolute pressure in the first processing stage is higher than second
Decision pressure in processing stage.
Particularly, the absolute pressure during the 1st processing stage is 5.0-6.0 × 10- 2mbar；2nd processing stage process
In absolute pressure be 3.0-6.0 × 10-3mbar。
Particularly, the treatment temperature of the 1st processing stage is -135~-145 DEG C, and glass treatment speed is 2-3m/min, excellent
It is selected as 3m/min；The treatment temperature of 2nd processing stage is 80-100 DEG C, and glass treatment speed is 2-3m/min, preferably 3m/
min。
Especially, the first hydrofuge, the processing time in degassing process stage are 40-50s, preferably 45s；Second hydrofuge takes off
The processing time in gas disposal stage is 80-100s, preferably 90s.
Particularly, step 2A is further included)：Institute is carried out again after treating the glass progress deionized water cleaning treatment of coating film treatment
The hydrofuge stated, degassing process.
Especially, content≤5 μ/cm/m of the deionized water mineral2；Temperature is 35-40 DEG C；Cleaning speed is
2-3m/min。
Particularly, the indoor absolute pressure of vacuum magnetic-control sputtering remains 2.0- during the step 3) coating film treatment
4.0×10-3Mbar, preferably 3.0 × 10-3mbar；The speed of plating is 0.6-0.8m/min, preferably 0.7m/min；Temperature
It is 80-100 DEG C.
Wherein, 2 plating of stainless steel alloy film described in step 3) point form.
Particularly, vacuum magnetic-control sputtering voltage is during first time plating during the plating of the stainless steel alloy film
550-556V, electric current 137.8-150.1A, power 50.1-60.1Kw；During the plating of the stainless steel alloy film
Vacuum magnetic-control sputtering voltage is 572-590V, electric current 133.6-140.2A, power 60.1- during secondary plating
70.1Kw。
Especially, in step 3) during the coating film treatment of first time plating stainless steel alloy film in vacuum magnetic-control sputtering room
Absolute pressure remain 2.0-4.0 × 10-3Mbar, preferably 3.0 × 10-3mbar；First layer stainless steel alloy described in plating
The speed of film is 0.6-0.8m/min, preferably 0.7m/min；Temperature is 80-100 DEG C.
Wherein, the indoor atmosphere of vacuum magnetic-control sputtering during the coating film treatment of the first time plating stainless steel alloy film
For oxygen and argon gas mixed gas.
Particularly, the ratio between volume of oxygen and argon gas is 2-20 in the atmosphere：1, preferably 2-10：1, further preferably
It is 2：1.
Especially, the flow of the oxygen is 1000sc/cm, and the flow of argon gas is 500sc/cm.
Particularly, the thickness of the first time plating of the first stainless steel alloy film is 4.8-5.2nm, preferably 5nm.
Especially, vacuum magnetic-control sputtering is indoor absolutely during the coating film treatment of the plating second layer stainless steel alloy film
2.0-4.0 × 10 are remained to pressure-6Mbar, preferably 3.0 × 10-3mbar；Second stainless steel alloy film described in plating
Speed is 0.6-0.8m/min, preferably 0.7m/min；Temperature is 80-100 DEG C.
Wherein, the indoor atmosphere of vacuum magnetic-control sputtering during the coating film treatment of second of plating stainless steel alloy film
Mixed gas for oxygen and argon gas.
Particularly, the ratio between volume of oxygen and argon gas is 2-60 in the atmosphere：1, preferably 2-30：1, further preferably
It is 2：1.
Especially, the flow of the oxygen is 1000sc/cm, and the flow of argon gas is 500sc/cm.
Particularly, the thickness of second of plating of the first stainless steel alloy film is 4.8-5.2nm, preferably 5nm.
Particularly, vacuum magnetic-control sputtering voltage is 664-670V during the coating film treatment of monocrystalline silicon membrane described in plating, electric
It flows for 32-50A, power 20.9-30.5Kw.
Particularly, the indoor absolute pressure of vacuum magnetic-control sputtering is kept during the coating film treatment of monocrystalline silicon membrane described in plating
For 2.0-4.0 × 10-6Mbar, preferably 3.0 × 10-3mbar；The speed of monocrystalline silicon membrane described in plating is 0.6-0.8m/min,
Preferably 0.7m/min；Temperature is 80-100 DEG C.
Wherein, the indoor atmosphere of vacuum magnetic-control sputtering is oxygen and argon during the coating film treatment of monocrystalline silicon membrane described in plating
The mixed gas of gas.
Particularly, the ratio between volume of oxygen and argon gas is 1-45 in the atmosphere：1, preferably 1：1.
Especially, the flow of the oxygen is 1200sc/cm, and the flow of argon gas is 1200sc/cm.
Particularly, vacuum magnetic-control sputtering voltage is 530-536V during the coating film treatment of titanium film described in plating, and electric current is
130.3-140.1A, power 60.1-70.1Kw.
Particularly, the indoor absolute pressure of vacuum magnetic-control sputtering remains during the coating film treatment of titanium film described in plating
2.0-4.0×10-6Mbar, preferably 3.0 × 10-3mbar；The speed of titanium film described in plating is 0.6-0.8m/min, preferably
0.7m/min；Temperature is 80-100 DEG C.
Wherein, the indoor atmosphere of vacuum sputtering is argon gas during the coating film treatment of titanium film described in plating.
Particularly, the flow of the argon gas is 500sc/cm.
Particularly, step 4) buffered is further included, the glass Jing Guo coating film treatment is conveyed from vacuum magnetic-control sputtering room
To pressure buffer room, the indoor pressure of buffering is gradually increased, until reaching normal pressure；It reduces and buffers indoor temperature, make interior
Temperature reaches 20-35 DEG C.
Another aspect of the present invention provides a kind of golden solar-control glazing being prepared according to the method described above.
The preparation method of the present invention and the product gold sunlight controlling coated glass prepared have the following advantages that：
1st, the golden solar-control glazing for preparing of the present invention using under vacuum conditions by magnetron sputtering glass table
Stainless steel alloy film, silicon fiml and titanium film are plated in face successively, and the composite membrane of glass surface is shown as golden under outdoor solar light, using valency
The cheap stainless steel alloy of lattice, silicon and titanium are target, overcome existing golden low radiation film coating glass generally use gold, silver, copper
Precious metals are waited as target, the defects of production cost costliness, low production efficiency, the life of golden solar-control glazing of the invention
Produce it is of low cost, conducive to promoting the use of for solar-control glazing.
2nd, golden solar-control glazing reflection colour prepared by the method for the present invention in gold, is set in the industries such as current building
Count the appearance color that teacher or owner appreciate, principal visual physical parameter is in L*=50~55, a*=0~2, b*=24~30 it
It is interior, it is colorful, beautiful, beautiful in outdoor in gold, it can be widely applied in various buildings, there is good decorative effect.
3rd, golden solar-control glazing prepared by the present invention, optical property technical parameter value meet GB/T18915.1-
2002《Coated glass part 1：Sunlight controlling coated glass》Standard, it is seen that luminous transmittance tolerance maximum value is small, far
Far below the 2.0% of national standard, reach and see that luminous transmittance tolerance maximum value is less than 0.5%；Color homogeneity is high, is less than
2.0CIELAB。
4th, golden solar-control glazing prepared by the present invention, it is seen that light transmission rate is less than 22%, outdoor visible reflectance
Higher than 35%, less than 31%, solar reflectance is higher than 36% for the transmitance of solar energy, suitable for build it is bright comfortable indoor and
Outdoor lighting environment；Meanwhile heat transfer coefficient winter is less than 4.8W/m2K, summer are less than 4.6W/m2K, shading coefficient (Sc) are low
In 0.47.Total transmitance of solar energy is relatively hot to increase less than 335w/m in 41%2, thermal property is good, can effective block sunlight
For heat to indoor radiation, energy-efficient performance is good, reduces energy consumption for cooling；Monolithic uses, and can reach good effect, save use into
This；Hollow glass is may be made as, control light energy-saving effect is more preferably.
5th, golden solar-control glazing of the invention can be obtained in preparation process by changing the thickness of each plated film film layer
The golden sunlight controlling coated glass of different optically and thermally performances is obtained, to adapt to market different demands.
Description of the drawings
Fig. 1 is the diagrammatic cross-section of the golden sunlight controlling coated glass of the present invention.
Reference numeral：1st, glass substrate；2nd, the first stainless steel alloy film；3rd, the second stainless steel alloy film；4th, monocrystalline silicon membrane；
5th, metal titanium membrane.
Specific embodiment
The present invention is further described below by embodiment, the advantages and features of the present invention will be with description and
It is apparent.But these embodiments are only exemplary, do not form any restrictions to the scope of the present invention.People in the art
Member it should be understood that without departing from the spirit and scope of the invention can to the details of technical solution of the present invention and form into
Row modifications or substitutions, but these modifications and replacement are each fallen in protection scope of the present invention.
As shown in Figure 1, the golden sunlight controlling coated glass of the present invention is successively by glass substrate 1, the first film layer 2, second
Film layer 3 and third membrane layer 4 form, and the first film layer 2 is fitted tightly on the surface of glass substrate 1, and the second film layer 3 is fitted tightly over
In first film layer 2, third membrane layer 4 is fitted tightly in the second film layer.First film layer is stainless steel alloy film, and the second film layer is single
Crystal silicon film, third membrane layer are metal titanium membrane.The thickness of first stainless steel alloy film is 9.6-10.4nm, preferably 10nm；Second
The thickness of single crystalline silicon film is 8.5-8.9nm, preferably 8.7nm；The thickness of third Titanium film layer is 20-23nm, preferably
21.5nm。
Embodiment 1
1st, target is sintered
In vacuum magnetron sputtering film plating machine (Xin Fuxing Glass Co., Ltd. of Fujian Province, model：XFXDM-01D) first,
Second, third, in the 4th target chamber, the target of pre-molding is sintered respectively in the corresponding target position of first to fourth target chamber,
In：It is >=99.5%, density is >=7.85g/cm that be sintered target on first, second target chamber target position, which be sintering purity,3, fusing point
For 1371-1398 DEG C of stainless steel (SST) alloy target material；Be sintered target on third target chamber target position be sintering purity for >=
99.99%, density is >=8.57g/cm3；Resistivity is≤0.005-0.20 μ Ω cm；Linear expansion coefficient is：(2~9) × 10-6K-1；Fusing point is 1410 DEG C of silicon target；Target of the sintering on the 4th target chamber target position is that sintering purity is >=99.99%, close
It spends for >=4.5g/cm3；Fusing point is 1668 DEG C of titanium target material, wherein, the sintering time of stainless steel and titanium is 30min, the sintering of silicon
Time is 200min；
Stainless steel (SST) alloy target material meets national standard《The stainless steel and refractory steel trade mark and chemical composition (GB/
T20878-2007)》The component requirements of middle 00Cr17Ni12Mo2；Silicon target meets national standard《Industrial silicon (GB/T2881-
2008)》The component requirements of middle level-one silicon；Titanium target material meets national standard《The titanium or titanium alloy trade mark and chemical composition (GB/
T3620.1-2007)》The component requirements of the industrial pure titaniums of TA2 in standard.
2nd, glass is cleaned
The float glass sheet that thickness is 6.0mm 2A) is placed in coating film on glass cleaning machine (German GTA companies production, type
Number：GTA01-M in), temperature is used as 37 DEG C, content≤5 μ/cm/m of minerals2Deionized water start the cleaning processing, clearly
Speed is washed as 4m/min；
Original sheet glass in the present invention is other than selecting the float glass sheet that thickness is 6mm, the glass of other thickness
Former piece is also applied for the present invention.Glass is cleaned using deionized water, the greasy dirt or other impurities of glass surface can not only be removed,
It avoids and cleans the problem of introducing other metal ions with tap water.
Processing 2B) is dried in the float glass after cleaning at 50 DEG C, wherein rate of drying is 4m/min, removes glass
Dry original sheet glass is made in the water droplet on glass surface.
3rd, hydrofuge, degassing process
Dry original sheet glass 3A) is sent to the first vacuum chamber of vacuum magnetron sputtering film plating machine with rollgang, to dry glass
Glass original piece carries out first time hydrofuge, degassing process, wherein first time hydrofuge, degassing process time for 45s, transmission speed is
0.7m/min；First time hydrofuge, degassing process temperature for -140 DEG C, absolute pressure is 5.0 × 10- 2mbar；
3B) the second vacuum chamber will be delivered to by the dry original sheet glass of first time hydrofuge, degassing process, carries out second and arrange
Wet, degassing process, wherein the time of second of hydrofuge, degassing process is 90s；Transmission speed is 0.7m/min；Second of hydrofuge,
The temperature of degassing process is 90 DEG C, and absolute pressure is 3.5 × 10-3Film glass to be plated is made in mbar.
In the multiple hydrofuge carried out to float glass sheet, during degassing process, treatment temperature gradually rises, relatively
Pressure reduces successively, eliminates the aqueous vapor and gas for being deposited on glass surface so that the clean surface of float glass to be coated increases
The adhesive force of glass surface and plated film interlayer is added, has made institute's film plating layer not easily to fall off；Meanwhile hydrofuge, degassing process three times, make to float
Method original sheet glass is in the environmental condition identical with during magnetron sputtering, convenient for the progress of subsequent operation, shortens coating film on glass
Time provides the efficiency of coating film on glass.
4th, coating film treatment
4A) open the power supply of the sputtering chamber of vacuum magnetron sputtering film plating machine, heating, make sputtering chamber (including first, second,
Third, the 4th target chamber) in temperature reach 80-100 DEG C, absolute pressure is reduced as 2.0-4.0 × 10-3(present invention is implemented mbar
Absolute pressure is with 3.0 × 10 in example-3Illustrated for mbar), film glass to be plated passes through first, second, third, fourth successively
Target chamber carries out magnetron sputtering film process；
4B) will successively it be sent with the transmission speed of 0.7m/min by film glass to be plated made from the 2nd hydrofuge, degassing process
Enter in first, second, third, fourth target chamber of film coating sputtering room, carry out coating film treatment, coated glass is made, technological parameter is such as
Shown in table 1, wherein：
Original sheet glass carries out first time plating stainless steel alloy coating film treatment in the first target chamber, and oxygen is passed through in the first target chamber
Gas and argon gas, the flow of oxygen are 1000sc/cm, the flow of argon gas for 500sc/cm (control the volume of oxygen and argon gas it
Than being 2:1), voltage 556V, electric current 137.8A, power 60.1Kw, the indoor absolute pressure of the first target for 2.0-4.0 ×
10-3Within mbar；The metallic atom of stainless steel (SST) alloy target material being sintered on first target chamber target position is sputtered from the surface of target
Go out, be deposited on the surface of float glass original sheet glass, the first time plated thickness of the first stainless steel alloy film layer is 5nm, is made
The first filming glass；
The first filming glass carries out second of plating stainless steel alloy coating film treatment in the second target chamber, leads in the second target chamber
Enter oxygen, argon gas, the flow of oxygen is 1000sc/cm, and the flow of argon gas (controls the volume of oxygen and argon gas for 500sc/cm
The ratio between be 2:1), voltage 572V, electric current 133.6A, power 60.1Kw, the control indoor absolute pressure of the second target are
2.0-4.0×10-3(selection 3.0 × 10-3) within mbar；Stainless steel (SST) alloy target material being sintered on second target chamber target position
Metallic atom is sputtered from the surface of target, is deposited on the surface of the first filming glass, and the second of the first stainless steel alloy film layer
Secondary plated thickness is 5nm, forms the first stainless steel alloy film layer that thickness is 10nm, the second coated glass is made；
Second coated glass carries out third time coating film treatment in third target chamber, and oxygen, argon gas, oxygen are passed through in third target chamber
The flow of gas is 1200sc/cm, and the flow of argon gas is that (it is 1 to control the ratio between volume of oxygen and argon gas to 1200sc/cm:1) it is, electric
It presses as 664V, electric current 32A, power 20.9Kw, it is 2.0-4.0 × 10 to control absolute pressure in third target chamber-3mbar(3.0
×10-3Mbar within)；The atom of monocrystalline silicon target on third target chamber target position is projected from the surface of target, is deposited on the second plating
The surface of film glass forms the third silicon film that thickness is 8.7nm, third coated glass is made；
Third coated glass carries out the 4th coating film treatment in the 4th target chamber, and argon gas is passed through in the 4th target chamber, oxygen
Flow is 0sc/cm, and the flow of argon gas is 500sc/cm, voltage 536V, electric current 140.1A, power 60.1Kw, control the
The indoor absolute pressure of four targets is 2.0-4.0 × 10-3mbar(3.0×10-3Mbar within)；It is sintered on 4th target chamber target position
The metallic atom of titanium target material is projected from the surface of target, is deposited on the surface of third coated glass, and it is 21.5nm's to form thickness
4th titanium film layer to get.
In stainless target, silicon target sputtering process with stainless steel, silicon oxidation occurs for coating film treatment step, oxygen instead
Should, generation oxidation stainless steel, silica, oxidation product not only increase the brightness of film layer so that stainless steel film layer with
Silicon film generates interference, and coated glass is made to be rendered as gold.
Wherein, first time plating stainless steel alloy film process to be formed on the surface of original sheet glass and be combined with glass surface
Firm foundations layer, and place mat is served to the formation of glass colour；Second of plating stainless steel alloy film process not only increases
The thickness of stainless steel film layer, and the brightness of glass colour is also improved, carry out magnetron sputtering coating stainless steel Alloy Plating twice
Film, it is excessive to solve power needed for a plated film, it is high to filming equipment requirement the problem of；Third time coating film treatment is in stainless steel membrane
Depositing monocrystalline silicon film is combined with stainless steel film layer on layer, makes glass in outdoor because reflex is in gold；At 4th plated film
Managing the titanium film deposited in single crystalline silicon film has excellent anticorrosive, crocking resistance, and protection has sputtered the film layer of formation,
Extend service life.
The technological parameter of coating film treatment is as shown in table 1 in embodiment 1.
The process parameter table of 1 embodiment of table, 1 coating film treatment
5th, buffered
4th coated glass is transported to from sputtering chamber in pressure buffer room, the indoor pressure of buffering and reduction is gradually increased
Indoor temperature is buffered, normal pressure is finally reached when buffering indoor pressure, when buffering indoor temperature reaches 20-35 DEG C, by the 4th plating
Film glass is discharged, and is put in storage to get to golden sunlight controlling coated glass.
Embodiment 2
1st, target is sintered
It is same as Example 1.
2nd, glass is cleaned
In addition to the deionized water temperature of cleaning is 35 DEG C, cleaning speed 3m/min, drying temperature is except 45 DEG C,
It is remaining same as Example 1；
3rd, hydrofuge, degassing process
Except the temperature of first time hydrofuge, degassing process is -135 DEG C, absolute pressure is 6.0 × 10- 2mbar；Second of row
Wet, degassing process temperature is 80 DEG C, and absolute pressure is 3.0 × 10- 3Except mbar, remaining is same as Example 1.
4th, coating film treatment
Other than the technological parameter of coating film treatment is with 1 difference of embodiment, remaining is same as Example 1, wherein at plated film
The technological parameter of reason is as shown in table 2.
The process parameter table of 2 embodiment of table, 2 coating film treatment
5th, buffered
It is same as Example 1.
Embodiment 3
1st, target is sintered
It is same as Example 1.
2nd, glass is cleaned
In addition to cleaning deionized water temperature be 40 DEG C, cleaning speed 5m/min, drying temperature be 55 DEG C except, remaining
It is same as Example 1；
3rd, hydrofuge, degassing process
In addition to the temperature of first time hydrofuge, degassing process is -145 DEG C, second of hydrofuge, degassing process temperature be 100
DEG C, absolute pressure is 6.0 × 10- 3Except mbar, remaining is same as Example 1.
4th, coating film treatment
Other than the technological parameter of coating film treatment is with 1 difference of embodiment, remaining is same as Example 1, wherein at plated film
The technological parameter of reason is as shown in table 3.
The process parameter table of 3 embodiment of table, 3 coating film treatment
5th, buffered
It is same as Example 1.
Reference examples 1
By monolithic gold sunlight controlling coated glass prepared by embodiment 1 be made structure for 6- gold solar-control glazing+
The hollow glass of 12Air+6glass is as reference examples 1.
Reference examples 2
By monolithic gold sunlight controlling coated glass prepared by embodiment 2 be made structure for 6- gold solar-control glazing+
The hollow glass of 12Air+6glass is as reference examples 2.
Reference examples 3
By monolithic gold sunlight controlling coated glass prepared by embodiment 3 be made structure for 6- gold solar-control glazing+
The hollow glass of 12-Air+6-glass is as reference examples 3.
Reference examples 4
Using the float glass sheet through glass pretreatment described in embodiment 1-3 as reference examples 4.
Reference examples 5
Structure is made as 6-glass+12-Air+ in the float glass sheet through glass pretreatment described in embodiment 1-3
The hollow glass of 6-glass reference examples 5 the most.
1 color of test example, wearability, resistance to acid and alkali experiment
According to GB/T2680-94《Building glass visible transmission ratio, the direct transmittance of sunlight, total solar energy transmittance,
Ultraviolet light projects the measure when in relation to glass pane parameter》And GB/T18915.2-2002《Coated glass part 1：Sunlight control
Coated glass processed》Standard is measured the color parameter of glass made from embodiment 1-3 and reference examples 1-5, and measurement result is such as
Shown in table 4,5.
4 color parameter measurement result of table
| Brightness value L* | Color a*Value | Color b*Value | Color homogeneity | Reflected colour aberration≤ | |
| Embodiment 1 | 52.63 | 0.29 | 24.87 | ≤1.5CIELAB | 2.5 |
| Embodiment 2 | 52.65 | 0.293 | 24.872 | ≤2.0CIELAB | 2.5 |
| Embodiment 3 | 52.62 | 0.289 | 24.868 | ≤2.0CIELAB | 2.5 |
| Reference examples 1 | 50.35 | -0.17 | 20.87 | ≤1.5CIELAB | 2.5 |
| Reference examples 2 | 50.52 | 0.47 | 19.76 | ≤2.0CIELAB | 2.5 |
| Reference examples 3 | 50.32 | 0.14 | 34.62 | ≤2.0CIELAB | 2.5 |
| Reference examples 4 | 43.13 | 0.32 | 37.82 | ≤3.0CIELAB | / |
| Reference examples 5 | 49.56 | 0.17 | 16.27 | ≤3.0CIELAB | / |
Table 5 is wear-resisting, resistance to acid and alkali, visible transmission are than measured performance parameter result
Golden solar control coated glass monolithic glass and its hollow glass, principal visual physical parameter prepared by the present invention exists
It is colorful, beautiful, beautiful in outdoor in gold within L*=50-55, a*=0-2, b*=24-30, it can be widely applied to each
In kind building.
2 optical property of test example is tested
The survey of optical property is carried out to glass made from embodiment 1-3 and reference examples 1-5 according to national standard GB/T2680-94
Fixed, test result is as shown in table 6,7.
6 optical performance test result of table
7 reference examples optical performance test result of table
The measurement result of table 6,7 shows：
1st, the visible light transmittance of the golden solar control coated glass monolithic glass of the present invention and hollow glass prepared therefrom is small
In 21.5%, the hollow glass that is prepared far below common monolithic glass and by simple glass, illustrating that the present invention can be controlled effectively can
See the injection of light, avoid indoor glare or excessively bright phenomenon；Reflectivity is more than 35% outside visible ray room, far above common monolithic glass
Glass and its hollow glass of preparation illustrate the coated glass of the present invention in a large amount of reflection room UV lights of outdoor energy；And its visible ray
Indoor reflection ratio and common monolithic glass and its hollow glass gap are little.
2nd, the golden solar control coated glass monolithic glass and hollow glass prepared therefrom, solar energy that prepared by the present invention are saturating
Rate is penetrated less than 31%, the hollow glass prepared far below common monolithic glass and by simple glass illustrates the sunlight control of the present invention
Glass processed is effectively controlled the injection of sunlight, reduces the amount of heat contained in sunlight and gets in；Its sunlight
Outdoor reflectivity is more than 36.8%, is reflected outside the sunlight room of hollow glass prepared far above simple glass and by simple glass
Rate illustrates that reflecting brightness is high outside the coated glass room of the present invention, and color is good；And sunshine absorptivity is more than 32.5%, is higher than
Simple glass and the hollow glass prepared by simple glass, illustrating the coated glass of the present invention can be absorbed heat by itself, be safeguarded
The ability of the light heat environment of indoor and outdoors is stronger.
3rd, the golden solar control coated glass monolithic glass and hollow glass prepared therefrom that prepared by the present invention, ultraviolet light
KShi transmitances, ISO transmitances and transmitance, substantially less than simple glass and by simple glass prepare hollow glass, it is ultraviolet
Line has the function of stronger sterilization colour fading, and transmittance is lower, shows that the ability of the coated glass blocking ultraviolet light of the present invention is strong, keeps away
Damage of the ultraviolet light to indoor article is exempted from.
4th, the optical property technical parameter value of metal solar-control glazing prepared by the present invention meets GB/T18915.1-
2002《Coated glass part 1：Sunlight controlling coated glass》Standard, it is seen that luminous transmittance tolerance maximum value is small, far
Far below the 2.0% of national standard, reach and see that luminous transmittance tolerance maximum value is less than 0.5%；Color homogeneity is high, is less than
2.0CIELAB。
Therefore, monolithic gold sunlight controlling coated glass of the present invention and the hollow glass for having its preparation are more advantageous to building light
Bright comfortable indoor and outdoors luminous environment, monolithic use can reach good effect, the using effect of hollow glass are made more
It is good.
3 Thermal Performance Test of test example
According to national standard GB/T2680-94《Building glass visible transmission ratio, the direct transmittance of sunlight, solar energy are always saturating
Penetrate the measure of ratio, ultraviolet light projection when in relation to glass pane parameter》Glass made from embodiment 1-3 and reference examples 1-5 is carried out
Thermal property is measured, and is calculated by WINDOW6.2 window curtain wall thermal property simulation softwards.
Experimental condition is：Winter is at night：- 18 DEG C of outdoor temperature, 21 DEG C, wind speed 5.5m/s of indoor temperature, without sunlight；Summer
Daytime：32 DEG C of outdoor temperature, 24 DEG C, wind speed 2.8m/s of indoor temperature, solar radiation intensity are 783w/ ㎡.Measurement result such as table
8th, shown in 9.
8 thermal performance test result of table
9 reference examples thermal performance test result of table
The measurement result of table 7,8 shows：
1st, the golden solar control coated glass monolithic glass energy saving for preparing of the present invention, either summer day be still
The energy saving in evening in winter is below common monolithic glass, and hollow glass prepared therefrom is also below by simple glass
The hollow glass of making shows that sunlight controlling coated glass prepared by the present invention can reduce different transfer of heat.
2nd, the golden solar control coated glass monolithic glass of the present invention and hollow glass prepared therefrom, shading coefficient are less than
0.47, total solar energy transmittance be less than 40.3%, substantially less than simple glass and by simple glass make hollow glass, hide
Positive coefficient and total solar energy transmittance are all the important references factors during building energy conservation calculates, and value is smaller, stop sunlight spoke
The performance penetrated is better, therefore shows the golden solar control coated glass monolithic glass of the invention prepared and hollow glass prepared therefrom
Solar energy can effectively be prevented to get in and be converted into thermal energy, so as to reduce energy consumption for cooling.
3rd, the relatively hot increasing of the golden solar control coated glass monolithic glass of the present invention and hollow glass prepared therefrom is less than
335W/m2, the substantially less than relatively hot increasing of simple glass and the hollow glass prepared by simple glass, relatively hot increasing is that synthesis is examined
Different transfer of heat and solar radiation to be considered on indoor influence, are obtained by glass and the sum of dispersed heat, relatively hot increment is smaller,
Then show that the heat got in by glass is fewer, more advantageously reduce energy consumption for cooling, golden sunlight of the invention control glass
The relatively hot increment of glass is small, shows that solar-control glazing prepared by the present invention has good energy-saving effect.
In short, monolithic gold sunlight controlling coated glass prepared by the present invention, more can than simple glass and its hollow glass
Effectively thermal energy is prevented to get in, while reducing energy consumption for cooling, reached energy-saving and environment-friendly purpose, monolithic use can reach
Good result is made better after hollow glass.
In conclusion golden sunlight controlling coated glass prepared by the present invention, compared with test example：Not only good appearance, color
It is color beautiful, there is decorative effect；And comfortable pleasant photo-thermal environment is advantageously formed, especially suitable for summer or southern temperature
Higher city.Monolithic, which uses or hollow glass is made, more satisfactory effect.
Claims (9)
1. a kind of preparation method of gold sunlight controlling coated glass, the step of progress including order below：
1) it is sintered target
Stainless steel alloy, silicon and titanium are sintered respectively on the target position of the vacuum sputtering room of glass film coating machine, it is spare；
2) pretreatment of glass
The glass of film process to be plated is placed under vacuum state, the glass for treating coating film treatment carries out hydrofuge, degassing process, reduces
Hydrofuge, degassing glass is made in the moisture content and gas of glass surface deposition；
3) coating film treatment
By hydrofuge, degassing glass be sent into glass film coating machine vacuum magnetic-control sputtering room in, hydrofuge, deaerate glass surface under
Plating stainless steel alloy film, monocrystalline silicon membrane and titanium film successively on and；Wherein：
2 plating of the stainless steel alloy film point form, and vacuum magnetic control splashes during first and second plating stainless steel alloy film
Indoor atmosphere is penetrated as oxygen and argon gas mixed gas, the ratio between volume of oxygen and argon gas is 2-20 during first time plating：
1, the ratio between volume of oxygen and argon gas is 2-60 during second of plating：1；
Mixed gas of the indoor atmosphere of vacuum magnetic-control sputtering for oxygen and argon gas during the coating film treatment of the monocrystalline silicon membrane,
The ratio between volume of oxygen and argon gas is 1-45：1；
The indoor atmosphere of vacuum sputtering is argon gas during the coating film treatment of the titanium film.
2. preparation method as described in claim 1, it is characterized in that the thickness of stainless steel alloy film layer described in step 3) is
9.6-10.4nm；The thickness of the single crystalline silicon film is 8.5-8.9nm；The thickness of the titanium film layer is 20-23nm.
3. preparation method as claimed in claim 1 or 2, it is characterized in that in a surface of glass plating institute successively from bottom to top
State stainless steel alloy film layer, single crystalline silicon film, titanium film layer.
4. preparation method as described in claim 1, it is characterized in that Vacuum Magnetic during first time plating stainless steel alloy film
Control sputtering voltage is 550-556V, electric current 137.8-150.1A, power 50.1-60.1kW；Second of plating coating stainless steel closes
Vacuum magnetic-control sputtering voltage is 572-590V, electric current 133.6-140.2A, power 60.1-70.1kW during golden film.
5. preparation method as described in claim 1, it is characterized in that in step 3) during the coating film treatment of plating monocrystalline silicon membrane
Vacuum magnetic-control sputtering voltage is 664-670V, electric current 32-50A, power 20.9-30.5kW.
6. preparation method as described in claim 1, it is characterized in that vacuum during the coating film treatment of plating titanium film in step 3)
Magnetron sputtering voltage is 530-536V, electric current 130.3-140.1A, power 60.1-70.1kW.
7. preparation method as described in claim 1, it is characterized in that hydrofuge described in step 2), degassing process are by glass to be coated
2 processing stages of glass point reduce the moisture content and gas of glass surface deposition, the obtained hydrofuge, degassing glass, wherein first
Absolute pressure in processing stage is higher than the absolute pressure in the second processing stage.
8. preparation method as claimed in claim 7, it is characterized in that the absolute pressure (5.0-6.0) during the 1st processing stage
×10- 2mbar；Absolute pressure during 2nd processing stage is (3.0-6.0) × 10-3mbar。
9. a kind of gold sunlight controlling coated glass, it is characterized in that being prepared according to such as any the methods of claim 1-8.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072158A (en) * | 1991-09-30 | 1993-05-19 | Ppg工业公司 | Heat treatable metal vacuum coating |
| CN101962271A (en) * | 2010-06-17 | 2011-02-02 | 张元胜 | Golden coated glass and preparation process thereof |
| CN202379890U (en) * | 2012-01-03 | 2012-08-15 | 揭阳市宏光镀膜玻璃有限公司 | Golden coated glass of special membrane system |
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2014
- 2014-05-05 CN CN201410185889.5A patent/CN105084776B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072158A (en) * | 1991-09-30 | 1993-05-19 | Ppg工业公司 | Heat treatable metal vacuum coating |
| CN101962271A (en) * | 2010-06-17 | 2011-02-02 | 张元胜 | Golden coated glass and preparation process thereof |
| CN202379890U (en) * | 2012-01-03 | 2012-08-15 | 揭阳市宏光镀膜玻璃有限公司 | Golden coated glass of special membrane system |
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Address after: 350314 Yan Dou village, Yuan Hong Industrial Zone, Fuqing City, Fuzhou, Fujian Patentee after: Xinfuxing Glass Industry Group Co., Ltd. Address before: Fuxing Industrial Park, 350314 Fujian city of Fuzhou province Fuqing City Yuanhong Investment Zone Patentee before: Fujian Xinfuxing Glass Co., Ltd. |