CN102219396A - Temperable gold low-emissivity coated glass and manufacturing method thereof - Google Patents
Temperable gold low-emissivity coated glass and manufacturing method thereof Download PDFInfo
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- CN102219396A CN102219396A CN2011100911078A CN201110091107A CN102219396A CN 102219396 A CN102219396 A CN 102219396A CN 2011100911078 A CN2011100911078 A CN 2011100911078A CN 201110091107 A CN201110091107 A CN 201110091107A CN 102219396 A CN102219396 A CN 102219396A
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Abstract
The invention relates to the technical field of glass manufacture and particularly provides temperable gold low-emissivity coated glass and a manufacturing method thereof for solving the technical problems that the existing gold coated glass products are difficult to temper, have poor appearance color, poor oxidation resistance, poor energy saving effect and the like. The glass base layer of the temperable gold low-emissivity coated glass provided by the invention is sequentially coated with the following film layers with specific thicknesses: a first silicon nitride film layer with a thickness of 19.1-41.9 nm, a first Ni-Cr alloy film layer with a thickness of 1.7-41.0 nm, a copper-indium alloy film layer with a thickness of 2.5-13.7 nm, a silver film layer with a thickness of 4.9-14.6 nm, a second nickel-chromium alloy film layer with a thickness of 1.7-6.3 nm and a second silicon nitride film layer with a thickness of 91.8-128.0 nm.
Description
Technical field
The present invention relates to glass technology for making field, but particularly be applied to the tempering golden low radiation film coating glass of special building cladding glass and windowpane etc.
Background technology
Existing golden coated glass mainly adopts low magnetron sputtering technology to carry out processing and manufacturing, the essence of this technology is to grow up on the basis of conventional DC (radio frequency) sputtering technology, it is by the constraint of magnetic field to lotus energy particle (mainly being electronics), improve the ionization level of gas molecule, can be under than higher vacuum state the thin-film material of very fast depositing high-quality.In brief, the ion that produces by electronics ionization of gas molecule (as typical A r+) bombardment target is realized thin film deposition.Promptly adopt particle or the particle beam irradiation solid surface that has kinetic energy more than tens electron-volts, can obtain the energy that projectile brings and break away from solid surface and itself have certain energy near the atom of solid surface, collision substrate deposition behind the flight certain distance and form film.The process that sputter takes place is as follows: projectile in entering the target material surface process with target atom generation elastic collision, the part energy of projectile has been passed to the atom of target, the energy that obtains when target atom has surpassed the constraint (potential barrier) of other atom formation that exists on every side, this atom from target lattice lattice point by knocking-on, when will collision mutually being taken place with other target particle in the particle flight course that bumps out, finally be deposited on substrate surface.
The golden coated glass that carries out processing and manufacturing by low magnetron sputtering technology mainly contains two classes:
First golden low radiation film coating glass (LOW-E) product, it mainly adopts medium target (medium layer), metal targets (protective layer), fine copper target, function target (low radiating layer) material to form the colden visual appearance tone according to certain sedimentary sequence and deposit thickness plated film on common float glass.Its production technique is: adopt magnetron sputtering mode plated film on common float glass, background vacuum pressure 5 * 10 under vacuum condition
-6More than the mbar, sputtering pressure 2 * 10
-3Mbar～8 * 10
-3Mbar deposits titanium oxide, copper, silver, nichrome, silicon nitride film layer successively on through the clean float glass that cleans, the deposit thickness of suitably regulating medium layer (silicon nitride) and functional layer (copper, silver) just reaches the colden visual appearance effect.Mainly there is following defective in golden low radiation film coating glass (LOW-E) product:
1. can not tempering thermal treatment.Promptly can not adopt tempering behind the big sheet glass plated film, but reduce production efficiency and strange land processibility.
2. outward appearance tone impure (presenting colour of loess tone).
3. antioxidant property is poor, and effectively the storage time is short.Put under the seal-packed situation of siccative, effective about 3 days of storage time, the time is long more, and the risk of rete oxidation then to occur just big more, increased quality control difficulty in the production process.
It two is golden heat reflection products, and it adopts high-purity silicon target, medium target material to form the colden visual appearance tone according to certain sedimentary sequence and deposit thickness plated film on common float glass.Its production technique is: adopt magnetron sputtering mode plated film on common float glass, background vacuum pressure condition 1 * 10 under vacuum condition
-5More than the mbar, sputtering pressure 4 * 10
-3Mbar～1 * 10
-2Mbar deposits stainless steel oxide, HIGH-PURITY SILICON, titanium oxide layer successively on through the clean float glass that cleans, suitably regulate medium layer (as stainless steel oxide) just deposit thickness reach the colden visual appearance effect.The subject matter of golden heat reflection product is that energy-saving effect is poor, summer U value=5.4, shading coefficient Sc=0.43.
U value and shading coefficient Sc are two important index weighing the energy-saving glass energy-saving effect, its implication is as follows: the U value refers under standard conditions, transmission heat from the glass assembly one side air of unit surface to the opposite side air in unit time, U value international unit is made as w/m
2.k, if the U value is big more, then energy-saving effect is poor more.U value=the 6.2w/m of common white glass
2.k; Shading coefficient Sc refers under the same conditions, sees through the solar radiant energy of glass and the ratio of the sun power that sees through the 3mm conventional clear glass.The solar radiant energy that sees through the 3mm conventional clear glass is 630w/m
2, shading coefficient=sun power direct radiation energy/630w/m
2What shading coefficient reflected is the heat transfer that direct solar radiation sees through glass.Shading coefficient is more little, and the performance of block sunlight direct radiation is good more.In actual application, often need to consider the lighting performance of buildings.Shading coefficient is a dimensionless parameters, the Sc=0.99 of the white glass of 6mm.
Summary of the invention
The present invention is intended to solve existing golden coated glass product and is difficult to that tempering is handled, technical problems such as the outward appearance tone is impure, oxidation-resistance is poor, energy-saving effect difference, but with provide a kind of tempering to handle, the outward appearance tone is pure, do that but oxidisability is good, the tempering golden low radiation film coating glass and the manufacture method thereof of good energy-conserving effect.
The objective of the invention is to be achieved through the following technical solutions.
But tempering golden low radiation film coating glass of the present invention, deposit the rete of following thickness on the glass-base successively, the first silicon nitride film layer 19.1-41.9 nm, the first nichrome rete 1.7-41.0 nm, copper and indium alloy rete 2.5-13.7 nm, silver film 4.9-14.6 nm, the second nichrome rete 1.7-6.3 nm, the second silicon nitride film layer 91.8-128.0 nm.
But tempering golden low radiation film coating glass of the present invention, wherein the copper and indium alloy rete adopts Cu-Al-Ni-In quad alloy target, and the weight percentage of four kinds of elements is respectively in the quad alloy target: Ni 1%～3%, Al 4.5%～7.5%, In 0.3%～1%, Cu 88.5%～94.2%.
But tempering golden low radiation film coating glass of the present invention, wherein glass is float glass.
But the manufacture method of tempering golden low radiation film coating glass of the present invention comprises the steps:
A) after the cleaning float glass basic unit, it is sent into vacuum chamber, vacuum degree in vacuum chamber is 7 * 10
-6More than the mbar;
B) control sputter vacuum tightness is 2 * 10
-3Mbar～1 * 10
-2Mbar deposits the rete of following thickness: the first silicon nitride film layer 19.1-41.0 nm, the first nichrome rete 1.7-41.0 nm, copper and indium alloy rete 2.5-13.7 nm, silver film 4.9-14.6 nm, the second nichrome rete 1.7-6.3 nm, the second silicon nitride film layer 91.8-128.0 nm successively in basic unit;
C) use online photometer measurement rete color parameter, and carry out the adjustment of thicknesses of layers, make color parameter and 18K gold approaching;
D) product that will finish the plated film debugging send the annealing furnace tempering.
But the manufacture method of tempering golden low radiation film coating glass of the present invention, wherein annealing furnace is full convection furnace in the steps d, and the bottom furnace temperature is 660 ℃～680 ℃, and the top furnace temperature is 680 ℃～700 ℃; Tempering heat-up time is 350～390S.
But the beneficial effect of the present invention's tempering golden low radiation film coating glass and manufacture method thereof:
1. appearance effect
But appearance color such as table one behind tempering 18K gold golden low radiation film coating glass (LOW-E) the product tempering:
Table one: 18K gold golden low radiation film coating glass appearance color
The implication of each parameter is as follows in the table one:
G: the glass surface of expression coated glass; F: the plated film face of expression coated glass; R*g: the reflectance value of expression coated glass glass surface; R*f: the reflectance value of expression coated glass face; L*g: the brightness of expression coated glass glass surface; L*f: the brightness of expression coated glass face; A*g, b*g: the color value of expression coated glass glass surface, (a*g is more just representing that color is red more, and a*g negative indication color more is green more; B*g is more just representing that color is yellow more, and b * g negative indication color more is blue more); A*f, b*f: the color value of expression coated glass face, (a*f is more just representing that color is red more, and a*f negative indication color more is green more; B*f is more just representing that color is yellow more, and b * f negative indication color more is blue more); T: the transmitance of expression coated glass; A*t, b*t: the color value that the expression coated glass sees through, (a*f is more just representing that color is red more, and a*f negative indication color more is green more; B*f is more just representing that color is yellow more, and b * f negative indication color more is blue more); E: the radiation value of expression coated glass.
2. energy-conservation situation
But the energy-conservation situation such as the table two of the imitative 18K gold of tempering golden low radiation film coating glass (LOW-E) product:
Table two: 18K gold golden low radiation film coating glass power save parameters
The implication of each parameter is as follows in the table two:
Visible light transmissivity: at visible light (wavelength: 380-780nm) in the scope, see through the percent value of glass light intensity; Visible reflectance: visible light (wavelength: 380-780nm) in the scope, the percent value of reflection of glass surface light intensity; Sun power transmitance: at solar spectrum (wavelength: 300-2500nm) in the scope, see through the percent value of UV-light, visible light and the near infrared light total energy of glass; Solar reflectance: solar spectrum (wavelength: 300-2500nm) in the scope, the percent value of the UV-light of reflection of glass surface, visible light and near infrared light total energy; U value: the heat transfer coefficient under the U.S. ASHRAE standard conditions.The value of heat transfer coefficient is relevant with test condition, with a kind of glass under different test conditions, the value difference of heat transfer coefficient.Shading coefficient: under the same terms, see through the total solar radiation energy of glass and the ratio of the total solar radiation energy that sees through the 3mm transparent glass.Shading coefficient is more little, and block sunlight radiating performance is good more.
3. productive rate promotes with the cost reduction and mainly shows following three aspects:
1) this novel product can adopt tempering behind the big sheet glass plated film, production efficiency than tempering after the plated film mode improved about 35%;
2) can carry out strange land processing, the trans-regional processing restriction of analogous products before having broken through;
3) process golden product according to order before this, can take to produce earlier the mode that receives orders again behind certain stock now, can shorten delivery date.
4. oxidation-resistance
Golden low radiation film coating glass (LOW-E) product puts under the prerequisite of siccative sealing effectively that be 3 days storage time before this, and the oxidized risk of long more its functional film layer of shelf-time is big more, and the quality control difficulty is big.But the oxidation-resistance of tempering 18K newly developed gold golden low radiation film coating glass (LOW-E) product significantly improves, show that it is 3 months that big plate coated glass is put siccative seal-packed effective storage time, this product can high temperature resistance environment (tempering thermal treatment) simultaneously.
Description of drawings
The film layer spectrum curve of Fig. 1 embodiment 1, appearance color, thicknesses of layers synoptic diagram
The film layer spectrum curve of Fig. 2 embodiment 2, appearance color, thicknesses of layers synoptic diagram
The film layer spectrum curve of Fig. 3 embodiment 3, appearance color, thicknesses of layers synoptic diagram
The film layer spectrum curve of Fig. 4 embodiment 4, appearance color, thicknesses of layers synoptic diagram
The film layer spectrum curve of Fig. 5 embodiment 5, appearance color, thicknesses of layers synoptic diagram
Embodiment
But the film layer structure of tempering 18K gold golden low radiation film coating glass (LOW-E) product is Glass/SiNx/NiCr+CuIn+Ag+NiCr/SiNx.In R﹠D process, adopt professional rete simulation software to carry out theoretical modeling, obtain the theoretic throat of each relevant rete, carry out the debugging of coating process then.The enforcement of coating process debugging is to carry out on the big area magnetron sputtering film device of Chinese Nan Bo group independent research.Float glass process Ben Tele cleaning machine enters vacuum chamber after cleaning and finishing in the process debugging process, successively deposited silicon nitride, nichrome, copper and indium alloy, silver, nichrome, silicon nitride film layer.The product that deposition is finished all retes adopts online photometer measurement color parameter.Changing Pattern according to color parameter of measuring and rete debugging carries out the adjustment of thicknesses of layers, debugs out and the approaching 6mm sample of 18K gold until final.Adopt test analytical instruments such as bench photometer, AE radiometer, portable colour photometer, shredder, Lambd 900 UV, visible light infrared spectrophotometers to test the glass face of acquisition products, face simultaneously, see through spectrum, import Window 5.2 in conjunction with the radiant ratio information of measuring and obtain relevant photo-thermal performance perameter with the Optics software for calculation.The product that plated film debugging is finished send annealing furnace to carry out tempering, and the main tempering parameter of annealing furnace is: full convection furnace, and the bottom furnace temperature is 660 ℃～680 ℃, and the top furnace temperature is 680 ℃～700 ℃, and tempering heat-up time is 350～390S.Adopt the performance of checking product behind the tempering in the same way behind the tempering, especially the photo-thermal behind the variable quantity of the appearance color before and after the tempering, emissivity change amount, rete adhesive ability, the tempering is learned performance perameter.The sample that is used for measure spectrum adopts the half tempered mode to prepare.According to the anti-appearance color of debugging before the tempering that pushes away of the variable quantity of appearance color behind the tempering, then carry out process debugging again, guarantee that the product behind the tempering reaches 18K gold colden visual appearance effect.
The major equipment instrument and the material that adopt in the R﹠D process:
Big area magnetron sputtering coating system, Benteler cleaning machine, online detection photometer, datacolor 550 (bench photometer), datacolar check (portable colour photometer), Lambda 900 (UV, visible light infrared spectrophotometer), AE radiometer, 5135 Abraser (shredder), concentration are that 0.1mol/L HCl solution, concentration are that 0.1mol/L NaOH solution, Window 5.2 and Optics photo-thermal are learned performance computation software.
At the product innovation of this exploitation, after its sputtering target material and film layer structure were determined, the core of decision product performance characteristics was debugging of coating process, promptly mainly by each relevant rete (functional layer CuIn, Ag; Medium layer SiNx; Protective layer NiCr) adjusting of deposit thickness finally reaches different appearance color, photo-thermal and learns performance perameter.As regulate its transmitance scope T=15%～40%, radiant ratio scope E=0.06～0.14 by thickness.The coating process aspect, the adjustable extent such as the table three of each relevant rete:
Table three: 18K gold golden low radiation film coating glass thicknesses of layers regulation range
With reference to accompanying drawing 1-5, principle of the present invention, effect and effect are illustrated by following embodiment.
Deposit the rete of following thickness on the glass-base successively, first silicon nitride film layer (1-SiNx) 19.7nm, the first nichrome rete (1-NiCr), 4.3 nm, copper and indium alloy rete (1-CuIn) 4.2nm, silver film (1-Ag) 6.9nm, the second nichrome rete (2-NiCr), 4.1 nm, second silicon nitride film layer (2-SiNx), 116.1 nm, its appearance color and the curve of spectrum are respectively shown in accompanying drawing one.
Deposit the rete of following thickness on the glass-base successively, first silicon nitride film layer (1-SiNx) 19.1nm, the first nichrome rete (1-NiCr), 6.4 nm, copper and indium alloy rete (1-CuIn) 2.5nm, silver film (1-Ag) 4.9nm, the second nichrome rete (2-NiCr), 6.8 nm, second silicon nitride film layer (2-SiNx), 116.1 nm, its appearance color and the curve of spectrum are respectively shown in accompanying drawing two.
Embodiment 3
Deposit the rete of following thickness on the glass-base successively, first silicon nitride film layer (1-SiNx) 19.1nm, the first nichrome rete (1-NiCr), 1.7 nm, copper and indium alloy rete (1-CuIn) 13.7nm, silver film (1-Ag) 14.6nm, second nichrome rete (2-NiCr) 1.7nm, second silicon nitride film layer (2-SiNx), 91.8 nm, its appearance color and the curve of spectrum are respectively shown in accompanying drawing three.
Embodiment 4
Deposit the rete of following thickness on the glass-base successively, first silicon nitride film layer (1-SiNx) 41.9nm, the first nichrome rete (1-NiCr), 1.7 nm, copper and indium alloy rete (1-CuIn) 2.9nm, silver film (1-Ag) 11.5nm, second nichrome rete (2-NiCr) 1.9nm, second silicon nitride film layer (2-SiNx), 128.0 nm, its appearance color and the curve of spectrum are respectively shown in accompanying drawing four.
Embodiment 5
Deposit the rete of following thickness on the glass-base successively, first silicon nitride film layer (1-SiNx) 23.1nm, the first nichrome rete (1-NiCr), 2.2 nm, copper and indium alloy rete (1-CuIn) 5.7nm, silver film (1-Ag) 9.5nm, second nichrome rete (2-NiCr) 2.3nm, second silicon nitride film layer (2-SiNx), 104.2 nm, its appearance color and the curve of spectrum are respectively shown in accompanying drawing five.
Claims (5)
1. but tempering golden low radiation film coating glass, it is characterized in that: deposit the rete of following thickness on the glass-base successively, the first silicon nitride film layer 19.1-41.9 nm, the first nichrome rete 1.7-41.0 nm, copper and indium alloy rete 2.5-13.7 nm, silver film 4.9-14.6 nm, the second nichrome rete 1.7-6.3 nm, the second silicon nitride film layer 91.8-128.0 nm.
2. but tempering golden low radiation film coating glass as claimed in claim 1, it is characterized in that: described copper and indium alloy rete adopts Cu-Al-Ni-In quad alloy target, and the weight percentage of four kinds of elements is respectively in the quad alloy target: Ni 1%～3%, Al 4.5%～7.5%, In 0.3%～1%, Cu 88.5%～94.2%.
3. but tempering golden low radiation film coating glass as claimed in claim 1 is characterized in that: described glass is float glass.
4. but the manufacture method of tempering golden low radiation film coating glass as claimed in claim 1 is characterized in that comprising the steps:
A) after the cleaning float glass basic unit, it is sent into vacuum chamber, vacuum degree in vacuum chamber is 7 * 10
-6More than the mbar;
B) control sputter vacuum tightness is 2 * 10
-3Mbar～1 * 10
-2Mbar deposits the rete of following thickness: the first silicon nitride film layer 19.1-41.0 nm, the first nichrome rete 1.7-41.0 nm, copper and indium alloy rete 2.5-13.7 nm, silver film 4.9-14.6 nm, the second nichrome rete 1.7-6.3 nm, the second silicon nitride film layer 91.8-128.0 nm successively in basic unit;
C) use online photometer measurement rete color parameter, and carry out the adjustment of thicknesses of layers, make color parameter and 18K gold approaching;
D) product that will finish the plated film debugging send the annealing furnace tempering.
5. but the manufacture method of tempering golden low radiation film coating glass as claimed in claim 4 is characterized in that: annealing furnace is full convection furnace in the steps d, and the bottom furnace temperature is 660 ℃～680 ℃, and the top furnace temperature is 680 ℃～700 ℃; Tempering heat-up time is 350～390S.
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Cited By (7)
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| CN102615877A (en) * | 2012-03-29 | 2012-08-01 | 江苏奥蓝工程玻璃有限公司 | Low-radiation coated glass capable of being toughened off line and production method thereof |
| CN103407225A (en) * | 2013-07-04 | 2013-11-27 | 威海蓝星玻璃股份有限公司 | Golden low-emissivity coated glass and manufacturing method thereof |
| CN103940755A (en) * | 2013-07-01 | 2014-07-23 | 北京物华天宝安全玻璃有限公司 | Angle test method for toughened double-silver film-coated glass and devices thereof |
| CN105084781A (en) * | 2014-05-05 | 2015-11-25 | 福建新福兴玻璃有限公司 | Golden low-radiation reflective glass and preparation method therefor |
| CN109612758A (en) * | 2018-12-17 | 2019-04-12 | 惠科股份有限公司 | Debugging method and debugging machine platform of coating equipment |
| US11053164B2 (en) * | 2017-12-08 | 2021-07-06 | Saint-Gobain Glass France | Solar control glass article |
| CN115807209A (en) * | 2022-11-23 | 2023-03-17 | 核工业西南物理研究院 | Coating structure applied to window film |
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| CN102615877A (en) * | 2012-03-29 | 2012-08-01 | 江苏奥蓝工程玻璃有限公司 | Low-radiation coated glass capable of being toughened off line and production method thereof |
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| CN105084781A (en) * | 2014-05-05 | 2015-11-25 | 福建新福兴玻璃有限公司 | Golden low-radiation reflective glass and preparation method therefor |
| US11053164B2 (en) * | 2017-12-08 | 2021-07-06 | Saint-Gobain Glass France | Solar control glass article |
| CN109612758A (en) * | 2018-12-17 | 2019-04-12 | 惠科股份有限公司 | Debugging method and debugging machine platform of coating equipment |
| CN109612758B (en) * | 2018-12-17 | 2021-04-02 | 惠科股份有限公司 | Debugging method and debugging machine platform of coating equipment |
| CN115807209A (en) * | 2022-11-23 | 2023-03-17 | 核工业西南物理研究院 | Coating structure applied to window film |
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Application publication date: 20111019 |