CN105084781A - Golden low-radiation reflective glass and preparation method therefor - Google Patents
Golden low-radiation reflective glass and preparation method therefor Download PDFInfo
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- CN105084781A CN105084781A CN201410185979.4A CN201410185979A CN105084781A CN 105084781 A CN105084781 A CN 105084781A CN 201410185979 A CN201410185979 A CN 201410185979A CN 105084781 A CN105084781 A CN 105084781A
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Abstract
The invention discloses golden low-radiation reflective glass and a preparation method therefor. The golden low-radiation reflective glass comprises a glass substrate, a first silicon-aluminium alloy film layer, a second nickel-chromium alloy film layer, a third silver film layer, a fourth nickel-chromium alloy film layer and a fifth silicon-aluminium metal film layer which are sequentially and compactly laminated from bottom to top. The preparation method comprises the following steps: 1) sintering a target material; 2) pre-treating a glass material; and 3) carrying out coating treatment. The low-radiation reflective glass disclosed by the invention is golden in the sun and can reach good decorating and energy-saving effects; the product can be processed in different places, so that the manufacturing cost of an enterprise is lowered; and the glass can be further manufactured to hollow glass, so that better light-controlling and energy-saving effects are achieved.
Description
Technical field
The coated glass that the present invention relates to a kind of coated glass preparation method and prepared by the method, particularly a kind of preparation method of low radiation coated glass and the low radiation coated glass of preparation thereof.
Background technology
Coated glass (Reflectiveglass) also claim reflecting glass.Coated glass is at one or more layers metal of glass surface coating, alloy or metal compound film, to change the optical property of glass, meets certain particular requirement.The different qualities of product pressed by coated glass, can be divided into following a few class: heat-reflecting glass, low emissivity glass (Low-E), electropane etc.
The production method of coated glass is a lot, as vacuum magnetic-control sputtering method, vacuum vapor deposition method, chemical Vapor deposition process and sol-gel method etc.Magnetron sputtering film glass utilizes magnetron sputtering technique can manufacture and design the complicated film system of multilayer, and can plate out multiple color on white glass substrate, the corrosion-resistant and wear resisting property of rete is better, is produce and use maximum technology at present.There is certain gap with magnetron sputtering plating glassy phase than all in the kind of vacuum evaporation coating film glass and quality, is progressively replaced by vacuum sputtering.Chemical Vapor deposition process on floatation glass production line, passes into reactant gases decompose at scorching hot glass surface, is deposited on the technology that glass surface forms coated glass equably.The equipment investment of the method is few, easy-regulating, and product cost is low, chemical stability good, can hot-work, is one of the most rising at present production method.Sol-gel method produces coated glass technique simply, and good stability, weak point is that product optical transmittance is too high, ornamental poor.
Magnetron sputtering method is the coated glass production technique that in current world wide, application at most, technique is the most stable, performance is best (radiant ratio E value≤0.12), kind is the abundantest, energy demand is relatively low.Because this production technique does not need to bundle use with floatation glass production line, namely float glass can be separated with glass coating technique and carry out, effectively reduce glass post-processing enterprise duplicate construction floatation glass production line, decrease CO2 emissions and relevant energy consumption.
The principle of magnetron sputtering plating adds a quadrature field and electric field between sputtered target pole (negative electrode) and anode, required rare gas element (being generally Ar gas) is filled with in high vacuum chamber, permanent magnet forms the magnetic field of 250 ~ 350 Gausses in target surfaces, with high-voltage electric field composition crossed electric and magnetic field.Under the effect of electric field, argon gas is ionized into positive ion and electronics, target is added with certain negative high voltage, the electronics sent from target pole increases by the effect in magnetic field and the ionization probability of working gas, highdensity plasma body is formed near negative electrode, Ar ion accelerates to fly to target surface under the effect of Lorentz force, and with very high speed bombardment target surface, on target, sputtered atom out flies to glass substrate and deposit film forming with higher kinetic energy disengaging target surface.
The heat-reflecting glass that current application is maximum and low emissivity glass adopt vacuum magnetic-control sputtering method and chemical Vapor deposition process to produce substantially.There are BOC Co. (U.S.) and Lai Bao company (Germany) in vacuum magnetic-control sputtering method device fabrication producer more famous in the world; There is MB Group Plc (Britain) etc. in Chemical Vapor Deposition Equipment producer.At present, China is number various schools of thinkers coated glass manufacturer, affect larger vacuum magnetic-control sputtering method manufacturer in the industry and have South China glass group company and Shanghai Sunlight coated glass company etc., there are Shandong blue star glass company and the Changjiang river float glass company etc. in chemical Vapor deposition process manufacturer.
Numerous to the PRODUCTION TRAITS of golden coated glass at present; such as publication number is that the application for a patent for invention of CN101244898A discloses a kind of golden low radiation film coating glass; glass list plated surface is covered with composite film; the outermost layer of composite film is a protective film; composite film comprises three-layer metal rete; wherein layer of metal rete is copper film layer, and one deck is silver film, and the layer of metal rete be close to below protective film is nichrome rete or titanium film layer.Its making method comprises cleaning, dry and plating, and plating is vacuum magnetic-control sputtering plating, dried glass is inserted the target room successively plating composite film of vacuum magnetron sputtering coating film equipment.The golden low radiation film coating glass that specific metallic copper is selected in this invention, silver makes for sputtering target material, bright in luster and easily adjustment, steady quality, make efficiency are high, but, what the method made is low radiation coated glass (LOW-E glass), only has higher reflectivity to the far infrared rays of wavelength in 4.5-25 micrometer range; Meanwhile, the low emissivity glass that this method makes contains easily oxidized silver film, and its oxidation not only can make the color of glass change, and this film system also can be made to lose Low emissivity and heat insulation performance, therefore can not use by monolithic.
Existing low radiation coated glass is light grey, light blue is main, the demand of building designers to building color cannot be met, and existing low radiation coated glass low visible light transmitance, high visible reflectivity, high solar specific absorption, be unfavorable for the attractive in appearance and energy-conservation of building, and larger to the potential safety hazard of product itself.Low radiation coated glass prepared by the present invention, overcomes above-mentioned defect, all has certain control action kou to wavelength region at the sunlight of 350-1800nm.The color of the golden low radiation film coating glass gold of current use has yellow gold and silver and copper on a functional, but research finds that the far infrared of copper controls bad, market progressively abandons copper as functional layer.Remaining only has gold and silver.Existing golden low radiation film coating glass employs the functional layer of copper and silver, and layers of copper easily variable color occurs in the life-time service process of low radiation coated glass.Meanwhile, the silver layer contained in golden low radiation film coating glass or layers of copper, can make golden thin out, then there are not the problems referred to above in sunlight controlling coated glass prepared by the present invention, the more bright-coloured bright eye of thus presented gold.
Summary of the invention
Primary and foremost purpose of the present invention provides a kind of preparation method of golden low radiation film coating glass and the golden low radiation film coating glass of preparation for above-mentioned existing coated glass technology of preparing Problems existing.Golden low radiation film coating glass prepared by the inventive method, in the sun in golden, can reach good decorative effect; Low, the outdoor visible reflectance of visible light transmissivity transmitance that is high, sun power is low, solar reflectance is high; And golden low radiation glass transition coefficient of the present invention is low, shading coefficient is low, thermal property is good, can effectively stop heat energy to enter indoor, reduces energy consumption for cooling, make double glazing, control light energy-saving effect is better.
For realizing object of the present invention, one aspect of the present invention provides a kind of golden low radiation film coating glass, comprising:
Glass substrate;
First rete, is positioned on glass substrate, and described first rete is silumin rete;
Second rete, be positioned on described first rete, described second rete is nichrome rete;
Third membrane layer, be positioned on described second rete, described third membrane layer is silver film;
4th rete, is positioned in described third membrane layer, and described 4th rete is nichrome rete;
5th rete, be positioned on described 4th rete, described 5th rete is silumin rete.
Wherein, the thickness of described first silumin rete is 32.0-40.0nm, is preferably 33.0-39.0nm; The thickness of described second nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm; The thickness of described 3rd silver film is 7.0-9.0nm, is preferably 7.8-8.2nm; The thickness of described 4th nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm; The thickness of described 5th silumin rete is 163.0-180.0nm, is preferably 167.0-176.0nm.
Particularly, superimposed described first silumin rete, the second nichrome rete, the 3rd silver film, the 4th nichrome rete, the 5th silumin rete successively from bottom to top on a described surface at glass substrate.
Wherein, coated glass face reflection colour value 60≤L
*≤ 65,0≤a
*≤ 2 ,-18≤b
*≤-20.
The present invention provides a kind of preparation method of golden low radiation film coating glass on the other hand, comprises the step that order is in this way carried out:
1) target is sintered
Silumin, nichrome, silver are sintered respectively on the target position of the vacuum sputtering room of glass film coating machine, for subsequent use;
2) pre-treatment of glass
Under the glass of process to be coated is placed in vacuum state, the glass treating coating film treatment carries out hydrofuge, degassed process, reduces moisture content and the gas of glass surface deposition, obtained hydrofuge, degassed glass;
3) coating film treatment
Vacuum magnetic-control sputtering hydrofuge, degassed glass being sent into glass film coating machine is indoor, plating first silumin rete, the second nichrome rete, the 3rd silver film, the 4th nichrome rete and the 5th silumin rete successively from bottom to top on the surface of hydrofuge, degassed glass.
Wherein, step 1) described in silumin select that sintering purity be>=99.5%, density is>=2.1g/cm
3, fusing point is sial (Si-Al) alloy of 580 DEG C, wherein Al content is 8-12 ± 2wt%, and all the other are Si; Described nichrome selection sintering purity is>=99.7%, density is>=8.5g/cm
3, fusing point is the nichrome of 1420 DEG C, wherein Cr content is 20 ± 1wt%, and all the other are Ni; Described silver selects sintering purity to be>=99.99%, and density is>=10.5g/cm
3; Fusing point is the silver metal of 960 DEG C.
Particularly, the sintering time of described silumin is 90min; The sintering time of described nichrome is 90min; The sintering time of described silver is 60min.
Especially, described silumin meets the component requirements of sial target in national sector standard JC/T2068-2011; Described nichrome meets the component requirements of nickel chromium triangle target in national sector standard JC/T2068-2011; Described silver meets the component requirements of silver-colored target in national sector standard JC/T2068-2011.
Wherein, step 2) described in hydrofuge, degassed process be the moisture content and the gas that reduce glass surface deposition treatment stage of glass to be coated being divided 2, obtained described hydrofuge, degassed glass, wherein first treatment stage in absolute pressure higher than second treatment stage in decision pressure.
Particularly, the 1st treatment stage process in absolute pressure be 5.0-6.0 × 10
-2mbar; The absolute pressure treatment stage of 2nd in process is 3.0-6.0 × 10
-3mbar.
Particularly, the treatment temp treatment stage of the 1st is-135 ~-145 DEG C, and glass treatment speed is 2-3m/min, is preferably 3m/min; The treatment temp treatment stage of 2nd is 80-100 DEG C, and glass treatment speed is 2-3m/min, is preferably 3m/min.
Especially, the first hydrofuge, degassed treatment stage treatment time be 40-50s, be preferably 45s; Second hydrofuge, degassed treatment stage treatment time be 80-100s, be preferably 90s.
Particularly, also step 2A is comprised): carry out described hydrofuge, degassed process again after the glass treating coating film treatment carries out washed with de-ionized water process.
Especially, the content≤5 μ/cm/m of described deionized water mineral
2; Temperature is 35-40 DEG C; Cleaning speed is 2-3m/min.
Particularly, step 3) absolute pressure of vacuum magnetic-control sputtering indoor remains 2.0-4.0 × 10 in described coating film treatment process
-3mbar, is preferably 3.0 × 10
-3mbar; The speed of plating is 1.8-2.0m/min, is preferably 1.8m/min; Temperature is 80-100 DEG C.
Wherein, step 3) described in the first silumin rete at twice plating form; Described 5th silumin rete divides four platings to form.
Particularly, in the plating process of described first silumin rete, in first time plating process, vacuum magnetic-control sputtering voltage is 440-450V, is preferably 443-450V; Electric current is 48-60A, is preferably 50-55A; Power is 17-21Kw, is preferably 17.8-20.0Kw; In second time plating process, vacuum magnetic-control sputtering voltage is 520-555V, is preferably 530-550V; Electric current is 35-45A, is preferably 38.0-42.0A; Power is 17.8-19.5Kw, is preferably 18.0-19.0Kw.
Wherein, in first, second plating process of described first silumin rete, the atmosphere of vacuum magnetic-control sputtering indoor is the mixed gas of nitrogen and argon gas.
Particularly, in atmosphere described in first, second plating process of described first silumin rete, nitrogen is 3-4:2 with the ratio of the volume of argon gas, is preferably 3:2.
Especially, the flow of described nitrogen is 900sc/cm, and the flow of argon gas is 600sc/cm.
Particularly, the first silumin film first time plating thickness be 17-20.5nm, be preferably 17.8-20.0nm.The thickness of the second time plating of the first silumin film is 14-19.5nm, is preferably 15.0-19.0nm.
Wherein, step 3) described in the second nichrome rete plating process in vacuum magnetic-control sputtering voltage be 310-330V, be preferably 320-325V; Electric current is 4.5-6.5A, is preferably 4.9-6.0A; Power is 1.5-2.5Kw, is preferably 1.8-2.0Kw.
Particularly, in the plating process of described second nichrome rete, the atmosphere of vacuum magnetic-control sputtering indoor is argon gas.
Especially, the flow of described argon gas is 1200sc/cm.
Particularly, the plated thickness of described second nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm.
Wherein, step 3) described in the 3rd silver film plating process in vacuum magnetic-control sputtering voltage be 400-425V, be preferably 410-420V; Electric current is 7-9A, is preferably 7.5-8.5A; Power is 3-4Kw, is preferably 3.2-3.5Kw.
Particularly, in the plating process of described 3rd silver film, the atmosphere of vacuum sputtering indoor is argon gas.
Especially, the flow of described argon gas is 1000sc/cm.
Particularly, the plated thickness of described 3rd silver film is 7-9nm, is preferably 7.8-8.2nm.
Wherein, step 3) described in the 4th nichrome rete plating process in vacuum magnetic-control sputtering voltage be 370-415V, be preferably 375-400V; Electric current is 5-6A, is preferably 5.2-5.7A; Power is 1.5-2.5Kw, is preferably 1.9-2.2Kw.
Particularly, in the plating process of described 4th nichrome rete, the atmosphere of vacuum magnetic-control sputtering indoor is argon gas.
Especially, the flow of described argon gas is 1200sc/cm.
Particularly, the plated thickness of described 4th nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm.
Wherein, step 3) described in the 5th silumin rete plating process in vacuum magnetic-control sputtering voltage in first time plating process be 655-670V, be preferably 665-670V; Electric current is 72-77A, is preferably 74-75A; Power is 41.5-44Kw, is preferably 42.5-43.5Kw; Vacuum magnetic-control sputtering voltage in the plating process of the 5th silumin rete in second time plating process is 590-620V, is preferably 600-612V; Electric current is 72-74A, is preferably 73-73.5A; Power is 41.5-44Kw, is preferably 42-43Kw; Vacuum magnetic-control sputtering voltage in the plating process of the 5th silumin rete in third time plating process is 680-700V, is preferably 690-695V; Electric current is 71-74A, is preferably 72-73A; Power is 41-44Kw, is preferably 42-43Kw; Vacuum magnetic-control sputtering voltage in the plating process of the 5th silumin rete in the 4th plating process is 660-680V, is preferably 670-675V; Electric current is 72-74A, is preferably 72.5-73A; Power is 39-44Kw, is preferably 40-43Kw.
Particularly, in first, second, third, fourth plating process of described 5th silumin rete, the atmosphere of vacuum magnetic-control sputtering indoor is the mixed gas of nitrogen and argon gas.
Especially, first time of described 5th silumin rete in atmosphere described in plating process nitrogen be 2-3:1 with the ratio of the volume of argon gas, be preferably 2:1.
Particularly, the flow of described nitrogen is 1100sc/cm, and the flow of argon gas is 550sc/cm.
Especially, in atmosphere described in the second time plating process of described 5th silumin rete, nitrogen is 17-18:11 with the ratio of the volume of argon gas, is preferably 18:11.
Particularly, the flow of described nitrogen is 900sc/cm, and the flow of argon gas is 550sc/cm.
Especially, in atmosphere described in the 3rd, the 4th plating process of described 5th silumin rete, nitrogen is 9-10:5 with the ratio of the volume of argon gas, is preferably 9:5.
Particularly, the flow of described nitrogen is 900sc/cm, and the flow of argon gas is 500sc/cm.
Particularly, the 5th silumin film first time plating thickness be 41-44nm, be preferably 43-44nm; The thickness of the second plating is 41-44nm, is preferably 42-44nm; The thickness of the 3rd plating is 41-44nm, is preferably 42-44nm; The thickness of the 4th plating is 38-45nm, is preferably 40-44nm.
Particularly, also comprise step 4) buffered, the glass through coating film treatment is delivered to pressure buffer indoor from vacuum magnetic-control sputtering room, improves the pressure in surge chamber gradually, until reach normal pressure; Reduce the temperature in surge chamber, make room temp reach 20-35 DEG C.
The present invention provides a kind of golden low radiation film coating glass be prepared from according to the method described above on the other hand.
The product golden low radiation film coating glass tool of preparation method of the present invention and preparation has the following advantages:
1, golden low radiation film coating glass prepared by the present invention adopt under vacuum conditions by magnetron sputtering at the surface of glass successively plating first silumin film, second nichrome film, 3rd silverskin, 4th nichrome film, 5th silumin film, the composite membrane of glass surface is shown as gold under outdoor solar light, adopt cheap silumin, nichrome, silver is target, overcome existing golden low radiation film coating glass and usually adopt a large amount of gold, silver, the noble metals such as copper are as target, production cost is expensive, the defect that production efficiency is low, the low production cost of golden low radiation film coating glass of the present invention, be beneficial to promoting the use of of low emissivity glass.
2, the golden low radiation film coating glass reflection colour that prepared by the inventive method is golden, it is the appearance color that in the industries such as current building, Designers or owner appreciate, its principal visual physical parameter is in L*=60 ~ 65, a*=0 ~ 2, within b*=-3 ~ 6, it in golden, dazzles coloured silk, beautiful, attractive in appearance in outdoor, can be widely used in, in various building, there is good decorative effect.
3, the golden low radiation film coating glass prepared of the present invention, its optical property technical parameter value meets the standard of GB/T18915.1-2002 " coated glass part 2: low radiation coated glass ", visible transmission is less than permissible variation maximum value, well below 3.0% of national standard, reach and see that optical transmittance permissible variation maximum value is lower than 0.5%; Color homogeneity is high, is less than 2.0CIELAB.
4, the double glazing that the golden low radiation film coating glass that prepared by the present invention is made, visible light transmissivity is less than 30%, and outdoor visible reflectance is higher than 29%, and the transmitance of sun power is lower than 26%, solar reflectance, higher than 35%, is suitable for building bright comfortable indoor and outdoors luminous environment; Meanwhile, its heat transfer coefficient winter is lower than 1.63W/m
2k, summer is lower than 1.537W/m
2k, shading coefficient (Sc) is lower than 0.36.Total transmitance of sun power is lower than 32%, and relatively hot increasing is lower than 240w/m
2, thermal property is good, can effectively block sunlight heat is to indoor radiation, and energy-efficient performance is good, reduces energy consumption for cooling, controls light energy-saving effect better.
5, golden low radiation film coating glass of the present invention can obtain the golden low radiation film coating glass of different optical and thermal property in preparation process by the thickness changing each plated film rete, also can be made into dissimilar double glazing, to adapt to the different demand in market.
6, the thermostability of golden low radiation film coating glass prepared of the present invention is high, can realize strange land heat treatment process, higher than the thermostability of solar-control glazing when Product processing.
Accompanying drawing explanation
Fig. 1 is the diagrammatic cross-section of golden low radiation film coating glass of the present invention.
Reference numeral: 1, glass substrate; 2, the first silumin rete; 3, the second nichrome rete; 4, the 3rd argent rete; 5, the 4th nichrome rete; 6, the 5th silumin rete.
Embodiment
Be further described the present invention below by embodiment, advantage and disadvantage of the present invention will be more clear along with description.But these embodiments are only exemplary, do not form any restriction to scope of the present invention.It will be understood by those skilled in the art that and can modify to the details of technical solution of the present invention and form or replace down without departing from the spirit and scope of the present invention, but these amendments and replacement all fall within the scope of protection of the present invention.
As shown in Figure 1, golden low radiation film coating glass of the present invention is made up of glass substrate 1, first rete 2, second rete 3, third membrane layer 4, the 4th rete 5, the 5th rete 6 successively, first rete 2 fits tightly on the surface of glass substrate 1, second rete 3 fits tightly on the first rete 2, third membrane layer 4 fits tightly on the second rete 3,4th rete 5 fits tightly in third membrane layer 4, and the 5th rete 6 fits tightly on the 4th rete 5.First rete is silumin film, and the second rete is nichrome film, and third membrane layer is golden silverskin, and the 4th rete is nichrome film, and the 5th rete is silumin film.The thickness of the first silumin rete is 32.0-40.0nm, is preferably 33.0-39.0nm; The thickness of the second nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm; The thickness of the golden silver film of tertiary membrane is 7-9nm, is preferably 7.8-8.2nm; The thickness of the 4th nichrome rete is 5.0-6.0nm, is preferably 5.3-5.7nm; The thickness of the 5th silumin rete is 163-180nm, is preferably 167-176nm.
Embodiment 1
1, target sintering
In vacuum magnetron sputtering film plating machine (Xin Fuxing Glass Co., Ltd. of Fujian Province, model: XFXDM-01D) the first to the 9th target chamber in, the target of pre-molding is sintered respectively on the corresponding target position of the first to the 9th target chamber, wherein: sinter at first, second, target on the six to nine target chamber target position for sintering purity be>=99.5%, density is>=2.1g/cm
3, fusing point is the silicon-aluminium alloy target material of 580 DEG C, wherein Al content is 8-12 ± 2wt%, and all the other are Si; In order to sinter, purity is>=99.7% to the target of sintering on the 3rd and the 5th target chamber target position, density is>=8.5g/cm
3, fusing point is the nichrome target of 1420 DEG C, wherein Cr content is 20 ± 1wt%, and all the other are Ni; The target of sintering on the 4th target chamber target position is>=99.99% for sintering purity, and density is>=10.5g/cm
3; Fusing point is the silver-colored target of 960 DEG C,
Wherein, the sintering time of silumin is 90min; The sintering time of nichrome is 90min; The sintering time of silver is 60min.
Silumin meets the component requirements of sial target in national sector standard JC/T2068-2011; Described nichrome meets the component requirements of nickel chromium triangle target in national sector standard JC/T2068-2011; Described silver meets the component requirements of silver-colored target in national sector standard JC/T2068-2011.
2, glass is cleaned
Be 2A) that the float glass sheet of 6.0mm is placed in glass coating cleaning machine (German GTA company produces, model: GTA01-M) by thickness, adopt temperature to be 37 DEG C, the content≤5 μ/cm/m of mineral substance
2deionized water carry out clean, cleaning speed is 4m/min;
Original sheet glass in the present invention is except the float glass sheet of 6mm except selecting thickness, and the original sheet glass of other thickness is also applicable to the present invention.Adopt washed with de-ionized water glass, greasy dirt or other impurity of glass surface can not only be removed, it also avoid the problem introducing other metal ions with tap water cleaning.
2B) float glass after cleaning is carried out drying treatment at 50 DEG C, wherein rate of drying is 4m/min, removes the water droplet of glass surface, obtained dry original sheet glass.
3, hydrofuge, degassed process
3A) dry original sheet glass rollgang is sent to the first vacuum chamber of vacuum magnetron sputtering film plating machine, carries out first time hydrofuge, degassed process to dry original sheet glass, the time of wherein hydrofuge, degassed process is for the first time 45s, and transmission speed is 0.7m/min; The temperature of hydrofuge, degassed process is-140 DEG C for the first time, and absolute pressure is 5.0 × 10
-2mbar;
3B) the dry original sheet glass through hydrofuge, degassed process is for the first time delivered to the second vacuum chamber, carries out second time hydrofuge, degassed process, the time of wherein second time hydrofuge, degassed process is 90s; Transmission speed is 1.8m/min; The temperature of second time hydrofuge, degassed process is 90 DEG C, and absolute pressure is 3.5 × 10
-3mbar, obtained glass to be coated;
In the present invention, glass transmission speed is described for 1.8m/min, and glass transmission speed is that 1.8-2.0m/min is all applicable to the present invention.
In the process of the repeatedly hydrofuge that float glass sheet is carried out, degassed process, treatment temp raises gradually, relative pressure reduces successively, especially the second hydrofuge, degassed treatment stage the corresponding prolongation treatment time, eliminate the aqueous vapor and gas that are deposited on glass surface, make the clean surface of float glass to be coated, add the sticking power between glass surface and coatings, make institute's coatings difficult drop-off; Meanwhile, 2 hydrofuges, degassed process, make float glass sheet be in the envrionment conditions identical with during magnetron sputtering, be convenient to the carrying out of subsequent operations, shorten the glass coating time, provide the efficiency of glass coating.
4, coating film treatment
4A) open the power supply of the sputtering chamber of vacuum magnetron sputtering film plating machine, heating, makes the temperature in sputtering chamber (comprising the first to the 9th target chamber) reach 80-100 DEG C, and absolute pressure reduces as 2.0-4.0 × 10
-3(in the embodiment of the present invention, absolute pressure is with 3.0 × 10 for mbar
-3mbar is that example is described), glass to be coated from first to the 9th target chamber carries out magnetron sputtering plating process successively;
4B) sent into successively in the first to the 9th target chamber of film coating sputtering room with the transfer rate of 1.8m/min by the glass to be coated obtained through 2 hydrofuges, degassed process, carry out coating film treatment, obtained coated glass, processing parameter is as shown in table 1, wherein:
Original sheet glass to be coated carries out first time plating silumin film process in the first target chamber, nitrogen and argon gas is passed in first target chamber, the flow of nitrogen is 900sc/cm, the flow of argon gas is 600sc/cm (ratio namely controlling the volume of nitrogen and argon gas is 3:2), voltage is 445V, electric current is 50A, and power is 18Kw, and the absolute pressure in the first target chamber is 2.0-4.0 × 10
-3within mbar; The atoms metal of the silicon-aluminium alloy target material that the first target chamber target position sinters goes out from the surface sputtering of target, is deposited on the surface of float glass original sheet glass, and the first time plated thickness of the first silumin rete is 18.0nm, obtained the first filming glass;
The first filming glass carries out the second time plating of the first silumin rete in the second target chamber, nitrogen, argon gas is passed in second target chamber, the flow of nitrogen is 900sc/cm, the flow of argon gas is 600sc/cm (ratio namely controlling the volume of oxygen and argon gas is 3:2), voltage is 532V, electric current is 39.6A, and power is 18.0Kw, and the absolute pressure controlled in the second target chamber is 2.0-4.0 × 10
-3mbar (selects 3.0 × 10
-3mbar) within; The atoms metal of the silumin alloy target material that the second target chamber target position sinters goes out from the surface sputtering of target, be deposited on the surface of the first filming glass, the second time plated thickness of the first silumin rete is the second silumin rete of 15.0nm, form the first silumin rete that thickness is 33.0nm, obtained second coated glass;
Second coated glass carries out third time coating film treatment in the 3rd target chamber, passes into argon gas in the 3rd target chamber, and the flow of argon gas is 1200sc/cm, and voltage is 322.7V, and electric current is 5.0A, and power is 1.8Kw, and controlling absolute pressure in the 3rd target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the nichrome target that the 3rd target chamber target position sinters penetrates from the surface of target, is deposited on the surface of the second coated glass, forms the second nichrome rete that thickness is 5.5nm, obtained 3rd coated glass;
3rd coated glass carries out the 4th coating film treatment in the 4th target chamber, passes into argon gas in the 4th target chamber, and the flow of argon gas is 1000sc/cm, and voltage is 410.0V, and electric current is 8.0A, and power is 3.2Kw, and the absolute pressure controlled in the 4th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atoms metal of the silver-colored target that the 4th target chamber target position sinters penetrates from the surface of target, is deposited on the surface of the 3rd coated glass, forms the 3rd silver film that thickness is 8nm, obtained 4th coated glass.
4th coated glass carries out the 5th coating film treatment in the 5th target chamber, passes into argon gas in the 5th target chamber, and the flow of argon gas is 1200sc/cm, and voltage is 375.8V, and electric current is 5.5A, and power is 2.0Kw, and the absolute pressure controlled in the 5th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the nichrome target that the 5th target chamber target position sinters penetrates from the surface of target, is deposited on the surface of the 4th coated glass, forms the 4th nichrome rete that thickness is 5.5nm, obtained 5th coated glass.
5th coated glass carries out the 6th coating film treatment in the 6th target chamber, nitrogen, argon gas is passed in 6th target chamber, the flow of nitrogen is 1100sc/cm, the flow of argon gas is 550sc/cm (ratio namely controlling the volume of oxygen and argon gas is 2:1), voltage is 666.0V, electric current is 74.3A, and power is 42.9Kw, and the absolute pressure controlled in the 6th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the silicon-aluminium alloy target material that the 6th target chamber target position sinters penetrates from the surface of target, be deposited on the surface of the 5th coated glass, silicon-aluminium alloy target material magnetron sputtering plating process in the 6th target chamber i.e. first time plating of the 5th silumin rete, the first time plated thickness wherein controlling the 5th silumin rete is 43.0nm, obtained 6th coated glass.
6th coated glass carries out the 7th coating film treatment in the 7th target chamber, nitrogen, argon gas is passed in 7th target chamber, the flow of nitrogen is 900sc/cm, the flow of argon gas is 550sc/cm (ratio namely controlling the volume of oxygen and argon gas is 18:11), voltage is 605.0V, electric current is 73.0A, and power is 43.0Kw, and the absolute pressure controlled in the 7th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the silicon-aluminium alloy target material that the 7th target chamber target position sinters penetrates from the surface of target, be deposited on the surface of the 6th coated glass, silicon-aluminium alloy target material magnetron sputtering plating process in the 7th target chamber i.e. second time plating of the 5th silumin rete, the second time plated thickness wherein controlling the 5th silumin rete is 43.0nm, obtained 7th coated glass.
7th coated glass carries out the 8th coating film treatment in the 8th target chamber, nitrogen, argon gas is passed in 8th target chamber, the flow of nitrogen is 900sc/cm, the flow of argon gas is 500sc/cm (ratio namely controlling the volume of oxygen and argon gas is 9:5), voltage is 693.0V, electric current is 72.4A, and power is 42.9Kw, and the absolute pressure controlled in the 8th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the silicon-aluminium alloy target material that the 8th target chamber target position sinters penetrates from the surface of target, be deposited on the surface of the 7th coated glass, silicon-aluminium alloy target material magnetron sputtering plating process in the 8th target chamber i.e. third time plating of the 5th silumin rete, the third time plated thickness wherein controlling the 5th silumin rete is 43.0nm, obtained 8th coated glass.
8th coated glass carries out the 9th coating film treatment in the 9th target chamber, nitrogen, argon gas is passed in 9th target chamber, the flow of nitrogen is 900sc/cm, the flow of argon gas is 500sc/cm (ratio namely controlling the volume of oxygen and argon gas is 9:5), voltage is 674.0V, electric current is 72.6A, and power is 42.0Kw, and the absolute pressure controlled in the 9th target chamber is 2.0-4.0 × 10
-3mbar (3.0 × 10
-3mbar) within; The atom of the silicon-aluminium alloy target material that the 9th target chamber target position sinters penetrates from the surface of target, be deposited on the surface of the 8th coated glass, silicon-aluminium alloy target material magnetron sputtering plating process in 9th target chamber i.e. the 4th plating of the 5th silumin rete, the 4th plated thickness wherein controlling the 5th silumin rete is 42.0nm, form the 5th silumin rete that thickness is 171.0nm, obtain the 9th coated glass.
Wherein, first time plating silumin rete process makes to be formed with glass surface in conjunction with firm foundations layer (i.e. the first time plating of the first silumin rete) on the surface of original sheet glass, and plays place mat effect to the formation of glass colour; Second time plating not only increases the thickness of sial rete, but also improves the brightness of glass colour, carries out twice magnetron sputtering plating silumin plated film, solves a plated film power demand excessive, require high problem to filming equipment; Nickel deposited Chrome metal powder rete on silumin rete, plays bottom provide protection to silver layer, prevents in the long-time use procedure of silver film and oxidizing reaction occurs, cause glass colour to change; The metal silverskin that nichrome rete deposits, this layer is the functional layer of low radiation coated glass, and nichrome film is matting layer, and protection silver layer, increases the brightness of product; Silverskin deposits the 4th nichrome rete, bottom provide protection is risen to silver layer, prevents in the long-time use procedure of silver film and oxidizing reaction occurs, cause glass colour to change; 4th nichrome film deposits the 5th silumin rete, and glass colour is interfered and rete protective effect; Wherein, the 5th silumin rete divides four platings to form, the 5th silumin rete mainly hard protective layer; crucial provide protection is played when product deep processing; gradation plating improves coating quality and thickness, also plays the interference effect of light simultaneously, makes the color of product more perfect.
In embodiment 1, the processing parameter of coating film treatment is as shown in table 1.
The process parameter table of table 1 embodiment 1 coating film treatment
5, buffered
9th coated glass is transported to pressure buffer indoor from sputtering chamber, the temperature improving the pressure in surge chamber gradually and reduce in surge chamber, when the pressure in surge chamber finally reaches normal pressure, when buffering room temp reaches 20-35 DEG C, 9th coated glass is discharged, warehouse-in, namely obtains golden low radiation film coating glass.
6, double glazing is made
The monolithic golden low radiation film coating glass of preparation is made the double glazing that structure is 6-golden low radiation film coating glass (glass)+12-Air+6-glass (white glass).
Embodiment 2
1, target sintering
Identical with embodiment 1.
2, glass is cleaned
Except the deionized water temperature of cleaning is 35 DEG C, cleaning speed is 3m/min, and drying temperature is outside 45 DEG C, and all the other are identical with embodiment 1;
3, hydrofuge, degassed process
Except the temperature of hydrofuge, degassed process is for the first time-135 DEG C, absolute pressure is 6.0 × 10
-2mbar; The temperature of second time hydrofuge, degassed process is 80 DEG C, and absolute pressure is 6.0 × 10
-3outside mbar, all the other are identical with embodiment 1.
4, coating film treatment
Except the processing parameter of coating film treatment is different from embodiment 1, all the other are identical with embodiment 1, and wherein the processing parameter of coating film treatment is as shown in table 2.
The process parameter table of table 2 embodiment 2 coating film treatment
5, buffered
Identical with embodiment 1.
6, double glazing is made
Identical with embodiment 1.
Embodiment 3
1, target sintering
Identical with embodiment 1.
2, glass is cleaned
Except cleaning deionized water temperature is 40 DEG C, cleaning speed is 5m/min, and drying temperature is outside 55 DEG C,
All the other are identical with embodiment 1;
3, hydrofuge, degassed process
Except first time hydrofuge, degassed process temperature be-145 DEG C, second time hydrofuge, degassed process temperature be 100 DEG C, absolute pressure is 3.0 × 10
-3outside mbar, all the other are identical with embodiment 1.
4, coating film treatment
Except the processing parameter of coating film treatment is different from embodiment 1, all the other are identical with embodiment 1, and wherein the processing parameter of coating film treatment is as shown in table 3.
The process parameter table of table 3 embodiment 3 coating film treatment
5, buffered
Identical with embodiment 1.
6, double glazing is made
Identical with embodiment 1.
Reference examples 1
To make through the pretreated float glass sheet of glass the double glazing example 1 in contrast that structure is 6-glass (white glass)+12Air+6-glass (white glass) described in embodiment 1-3.
Reference examples 2
By described in embodiment 1-3 through the pretreated float glass sheet of glass example 2 in contrast.
Test example 1 color, wear resistance, radiant ratio are tested
According to GB/T2680-94 " projection of building glass visible transmission ratio, the direct transmittance of sunlight, total solar energy transmittance, ultraviolet is when about the mensuration of window glass parameter " and GB/T18915.2-2002 " coated glass part 2: low radiation coated glass " standard, measure the color parameter of the glass that embodiment 1-3 and reference examples 1-5 obtains, measurement result is as shown in table 4.
Table 4 measured performance parameter result
Golden low radiation plated film monolithic glass prepared by the present invention and double glazing thereof, its principal visual physical parameter is within L*=60-65, a*=0-2, b*=-20--15, and it in golden in outdoor, dazzled coloured silk, beautiful, attractive in appearance, can be widely used in various building.
Test example 2 optical property is tested
According to GB/T2680-94 " projection of building glass visible transmission ratio, the direct transmittance of sunlight, total solar energy transmittance, ultraviolet is when about the mensuration of window glass parameter ", the glass that embodiment 1-3 and reference examples 1-5 obtains is carried out to the mensuration of optical property, test result is as shown in table 5.
Table 5 optical performance test result
The measurement result of table 5 shows:
1, the visible light transmissivity of double glazing that the present invention is prepared by golden low radiation film coating glass is less than 29.11%, far below common monolithic glass and the double glazing prepared by simple glass, illustrate that the present invention can effectively control injecting of visible ray, avoid indoor glare or cross bright phenomenon; The outdoor reflectivity of visible ray higher than 30.17%, far above the double glazing of common monolithic glass and preparation thereof, illustrate coated glass of the present invention outdoor can a large amount of reflection room UV light; And its visible ray indoor reflection than with common monolithic glass and double glazing gap little.
Double glazing prepared by the golden low radiation film coating glass that 2, prepared by the present invention, its solar energy transmission is lower than 25.31%, far below common monolithic glass and the double glazing prepared by simple glass, illustrate that solar-control glazing of the present invention effectively controls injecting of sunlight, decrease the amount of heat contained in sunlight and enter indoor; The outdoor reflectivity of its sunlight is greater than 35.56%, and far above simple glass and the outdoor reflectivity of sunlight of double glazing prepared by simple glass, illustrate that the outdoor reflecting brightness of coated glass of the present invention is high, color is good; And sunlight specific absorption is higher than 39.13%, far away higher than simple glass and the double glazing prepared by simple glass, illustrate that coated glass of the present invention by the regulation and control of self heat, can safeguard that the ability of the light heat environment of indoor and outdoors is stronger.
Double glazing prepared by the golden low radiation film coating glass that 3, prepared by the present invention, its ultraviolet KShi transmitance, ISO transmitance and transmitance, all remarkable in simple glass and the double glazing prepared by simple glass, ultraviolet has stronger sterilization and to fade function, transmittance is lower, show that the ability of coated glass shielding of ultraviolet of the present invention is strong, avoid the damage of ultraviolet to indoor article.
4, the optical property technical parameter value of golden low radiation film coating glass that prepared by the present invention meets the standard of GB/T18915.2-2002 " coated glass part 2: low radiation coated glass ", visible transmission is less than permissible variation maximum value, well below 2.0% of national standard, reach visible transmission than permissible variation maximum value lower than 0.5%; Color homogeneity is high, is less than 2.0CIELAB.
Therefore, the golden sunlight controlling coated glass of monolithic of the present invention and the double glazing having it to prepare more are conducive to building bright comfortable indoor and outdoors luminous environment, and monolithic uses can reach good effect, and the result of use making double glazing is better.
Test example 3 Thermal Performance Test
The glass obtained embodiment 1-3 and reference examples 1-2 carries out the mensuration of thermal property.
Measure according to GB GB/T2680-94 " projection of building glass visible transmission ratio, the direct transmittance of sunlight, total solar energy transmittance, ultraviolet is when about the mensuration of window glass parameter ", calculated by WINDOW6.2 window curtain wall thermal property simulation software.
Test conditions is: evening in winter: external temperature-18 DEG C, room temp 21 DEG C, and wind speed 5.5m/s, without sunlight; Summer day: external temperature 32 DEG C, room temp 24 DEG C, wind speed 2.8m/s, solar radiation intensity is 783w/ ㎡.Measurement result is as shown in table 6.
Table 6 thermal performance test result
The measurement result of table 6 shows:
The energy saving of double glazing prepared by the golden low radiation film coating glass that 1, prepared by the present invention, be no matter that the energy saving in summer day or evening in winter all examines glass lower than common monolithic glass with in being prepared by simple glass, show that sunlight controlling coated glass prepared by the present invention can reduce different transfer of heat.
2, the double glazing prepared of golden low radiation film coating glass of the present invention, its shading coefficient is less than 0.363; Total solar energy transmittance is lower than 31.74%, all remarkable in simple glass and the double glazing that made by simple glass, shading coefficient and total solar energy transmittance are all the important references factors during building energy conservation calculates, its value is less, stop that the performance of solar radiation is better, therefore show that golden low radiation film coating glass prepared by the present invention and double glazing prepared therefrom effectively can stop sun power to enter indoor and be converted into heat energy, thus reduce energy consumption for cooling.
3, the relatively hot increasing of double glazing that prepared by golden low radiation film coating glass of the present invention is less than 242W/m
2significantly lower than simple glass and the relatively hot increasing of double glazing prepared by simple glass, relatively hot increasing considers different transfer of heat and solar radiation to the impact of indoor, obtained and dispersed heat sum by glass, relatively hot increment is less, then show to enter indoor heat by glass fewer, be more conducive to reducing energy consumption for cooling, the relatively hot increment of golden solar-control glazing of the present invention is little, shows that solar-control glazing prepared by the present invention has good energy-saving effect.
In a word, the golden sunlight controlling coated glass of monolithic prepared by the present invention, more can effectively stop heat energy to enter indoor than simple glass and double glazing thereof, while reducing energy consumption for cooling, reach the object of energy-conserving and environment-protective, monolithic uses can reach good result, and after making double glazing, effect is better.
In sum, golden sunlight controlling coated glass prepared by the present invention, than test example: not only good looking appearance, color is beautiful, has decorative effect; And be conducive to forming comfortable pleasant photo-thermal environment, be specially adapted to summer or the higher city of southern temperature.Monolithic uses or makes double glazing all more satisfactory effect.
Claims (10)
1. a golden low radiation film coating glass, is characterized in that, comprising:
Glass substrate (1);
First rete (2), is positioned on glass substrate, and described first rete is silumin rete;
Second rete (3), be positioned on described first rete, described second rete is nichrome rete;
Third membrane layer (4), be positioned on described second rete, described third membrane layer is silver film;
4th rete (5), is positioned in described third membrane layer, and described 4th rete is nichrome rete;
5th rete (6), be positioned on described 4th rete, described 5th rete is silumin rete.
2. coated glass as claimed in claim 1, is characterized in that the thickness of described first silumin rete is 32.0-40.0nm; The thickness of described second nichrome rete is 5.0-6.0nm; The thickness of described 3rd silver film is 7.0-9.0nm; The thickness of described 4th nichrome rete is 5.0-6.0nm; The thickness of described 5th silumin rete is 163.0-180.0nm.
3. coated glass as claimed in claim 1 or 2, to is characterized in that on a surface of glass substrate (1) from bottom to top superimposed described first silumin rete, the second nichrome rete, the 3rd silver film, the 4th nichrome rete, the 5th silumin rete successively.
4. a preparation method for golden low radiation film coating glass, comprises the step that following order is carried out:
1) target is sintered
Silumin, nichrome, silver are sintered respectively on the target position of the vacuum sputtering room of glass film coating machine, for subsequent use;
2) pre-treatment of glass
Under the glass of process to be coated is placed in vacuum state, the glass treating coating film treatment carries out hydrofuge, degassed process, reduces moisture content and the gas of glass surface deposition, obtained hydrofuge, degassed glass;
3) coating film treatment
Vacuum magnetic-control sputtering hydrofuge, degassed glass being sent into glass film coating machine is indoor, plating first silumin rete, the second nichrome rete, the 3rd silver film, the 4th nichrome rete and the 5th silumin rete successively from bottom to top on the surface of hydrofuge, degassed glass.
5. preparation method as claimed in claim 4, is characterized in that step 3) described in the first silumin rete at twice plating form.
6. preparation method as claimed in claim 5, to it is characterized in that in the plating process of described first silumin rete that in first time plating process, vacuum magnetic-control sputtering voltage is 440-450V, electric current is 48-60A, and power is 17.0-21.0Kw; In second time plating process, vacuum magnetic-control sputtering voltage is 520-555V, and electric current is 35-45A, and power is 17.8-19.5Kw.
7. the preparation method as described in claim 4 or 5, is characterized in that step 3) described in the second nichrome rete plating process in vacuum magnetic-control sputtering voltage be 310-330V, electric current is 4.5-6.5A, and power is 1.5-2.5Kw; In the plating process of described 3rd silver film, vacuum magnetic-control sputtering voltage is 400-425V, and electric current is 7.0-9.0A, and power is 3.0-4.0Kw.
8. the preparation method as described in claim 4 or 5, is characterized in that described 5th silumin rete divides four platings to form.
9. the preparation method as described in claim 4 or 5, it is characterized in that step 2) described in hydrofuge, degassed process be the moisture content and the gas that reduce glass surface deposition treatment stage of glass to be coated being divided 2, obtained described hydrofuge, degassed glass, wherein first treatment stage in absolute pressure higher than second treatment stage in decision pressure.
10. preparation method as claimed in claim 9, absolute pressure 5.0-6.0 × 10 treatment stage of it is characterized in that the 1st in process
-2mbar; The absolute pressure treatment stage of 2nd in process is 3.0-6.0 × 10
-3mbar.
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| CN114656163A (en) * | 2022-03-31 | 2022-06-24 | 新福兴玻璃工业集团有限公司 | Functional double-silver low-emissivity coated glass and preparation method thereof |
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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. |