CN102372447B - Low emissivity glass containing silver and manufacture method - Google Patents
Low emissivity glass containing silver and manufacture method Download PDFInfo
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- CN102372447B CN102372447B CN201010261823.1A CN201010261823A CN102372447B CN 102372447 B CN102372447 B CN 102372447B CN 201010261823 A CN201010261823 A CN 201010261823A CN 102372447 B CN102372447 B CN 102372447B
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Abstract
The invention discloses a low emissivity glass containing silver, a structure of a film layer successively comprises a glass substrate, a base layer dielectric combination layer, a first silver layer, a first blocking layer, a first interlayer dielectric combination layer, a second silver layer, a second blocking layer, a second interlayer dielectric combination layer, a third silver layer, a third blocking layer, a third interlayer dielectric combination layer, a fourth silver layer, a fourth blocking layer, an upper layer dielectric combination layer. The glass containing silver has the advantages of low emissivity, high visible light transmittance, no interference color appearance, high selection coefficient and good energy saving effect; the unique film layer structure has the advantages of good weatherability, difficult shedding and difficult oxidation, and can be widely popularized and applied to vehicle glass and civil architecture glass. The invention also provides a method for manufacturing low emissivity glass containing silver.
Description
[technical field]
The present invention relates to special glass field, relate in particular to a kind of silver-containing low emissivity glass and manufacture method thereof.
[background technology]
Low emissivity glass is a kind of at glass surface deposition one deck infrared reflection material, visible ray in sunlight can be seen through, again as infrared reflection mirror, the special glass that the infrared rays in sunlight is foreclosed and object secondary rays heat reflection gone back simultaneously.By using low emissivity glass, can reach the effect of controlling sunlight, save energy, heat regulating and controlling and improving environment.
In traditional low emissivity glass course of processing, in order to realize good U value and to select coefficient Lsg, just must increase the radiant ratio that silver thickness in rete reduces glass rete, to obtain desirable selection coefficient, but increase silver thickness, just mean that visible light transmissivity reduces, appearance color presents interference color, affect the use of glass.
[summary of the invention]
Based on this, be necessary to provide the silver-containing low emissivity glass that a kind of visible light transmissivity is high, outward appearance does not present interference color.
Meanwhile, be also necessary to provide the manufacture method that a kind of visible light transmissivity is high, outward appearance does not present the silver-containing low emissivity glass of interference color.
A silver-containing low emissivity glass, film layer structure is followed successively by: glass substrate, basic unit's dielectric combination layer, the first silver layer, the first blocking layer, the first interlayer dielectric combination layer, the second silver layer, the second blocking layer, the second interlayer dielectric combination layer, the 3rd silver layer, the 3rd blocking layer, the 3rd interlayer dielectric combination layer, the 4th silver layer, the 4th blocking layer, upper strata dielectric combination layer.
Preferably, basic unit's dielectric combination layer, the first interlayer dielectric combination layer, the second interlayer dielectric combination layer, the 3rd interlayer dielectric combination layer, upper strata dielectric combination layer are by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations; The first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th blocking layer are by Ni, Cr, NiCrO
xand NiCrN
xin one or more formations.
Preferably, basic unit's dielectric combination layer thickness is 25～27nm; The first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th barrier layer thickness are 0.25～0.3nm; The first interlayer dielectric combination layer thickness is 68～69nm; The second interlayer dielectric combination layer thickness is 70～71nm; The 3rd interlayer dielectric combination layer thickness is 72～73nm; Upper strata dielectric combination layer thickness is 24～27nm.
Preferably, in four silver thickness, require the first silver thickness to be less than that the second silver layer, the second silver thickness are less than the 3rd silver layer, the 3rd silver thickness is less than the 4th silver layer.Four layers of silver thickness summation are about 43nm～47nm, and its each silver thickness relation meets product appearance color as the color value scope in following table:
| Monolithic appearance color | Glass surface reflected colour | Rete face reflected colour | Transmitted colour |
| Y | Be less than 7 | Be less than 8 | Be greater than 70 |
| L* | Be less than 32 | Be less than 34 | Be greater than 87 |
| a* | -0.5～-1.8 | 1.2～1.8 | -6.0～-5.0 |
| b* | -3.5～-4.5 | -4.5～-5.5 | -1.0～2.0 |
Preferred, the first silver thickness is 7～8nm; The second silver thickness is 11～12nm; The 3rd silver thickness is 12～13nm; The 4th silver thickness is 13～14nm.
Preferably, upper strata dielectric combination layer comprises the first upper strata dielectric combination layer being deposited on the 4th blocking layer and is deposited on the second upper strata dielectric combination layer in the first upper strata dielectric combination layer; The first upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations; The second upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations.
Preferred, first, second upper strata dielectric combination layer forms with the stack of differing materials alternating sputtering conventionally, and object is to make rete possess antireflective coating and low absorptivity.
Particularly preferred, the second upper strata dielectric combination layer at least comprises TiO
2, SiO
2and Si
3n
4in a kind of.
The thickness of the first upper strata dielectric combination layer is 15～16nm; The thickness of the second upper strata dielectric combination layer is 9～11nm.
Sputtering ZnS nO
x, NiCrO
x, NiCrN
xin chemical formula etc. incomplete oxidation thing or full oxide, incomplete nitride or complete nitride, x is greater than 0, and the maximum value that can get is metal or nonmetal actual value while adding certain oxygen or nitrogen flow (generally adding oxygen or nitrogen gas stream value to be equivalent to 15 times of this target sputtering power) rear oxidation.
A manufacture method for silver-containing low emissivity glass, comprises the step that deposits successively each rete, specific as follows:
S1, cleaning glass substrate, the dry magnetron sputtering area that is placed on;
S2, intermediate frequency power supply add rotating cathode sputtering sedimentation basic unit dielectric combination layer;
S3, direct supply add pulse sputtering sedimentation the first silver layer;
S4, direct supply add pulse sputtering sedimentation the first blocking layer;
S5, intermediate frequency power supply add rotating cathode sputtering sedimentation the first interlayer dielectric combination layer;
S6, direct supply add pulse sputtering sedimentation the second silver layer;
S7, direct supply add pulse sputtering sedimentation the second blocking layer;
S8, intermediate frequency power supply add rotating cathode sputtering sedimentation the second interlayer dielectric combination layer;
S9, direct supply add pulse sputtering sedimentation the 3rd silver layer;
S10, direct supply add pulse sputtering sedimentation the 3rd blocking layer;
S11, intermediate frequency power supply add rotating cathode sputtering sedimentation the 3rd interlayer dielectric combination layer;
S12, direct supply add pulse sputtering sedimentation the 4th silver layer;
S13, direct supply add pulse sputtering sedimentation the 4th blocking layer;
S14, intermediate frequency power supply add rotating cathode sputtering sedimentation upper strata dielectric combination layer.
Preferably, during deposition plating, coating wire configuration keeping system background vacuum vacuum tightness is 3 * 10
-6dry molecular pump more than mbar; The contiguous compartment position of silver target disposes for absorbing the cryopump of moisture.
Preferably, it is to carry out in argon nitrogen or argon oxygen atmosphere that intermediate frequency power supply adds rotating cathode sputter, and frequency is 35～45kHz, and power is 30～50kw; Wherein, intermediate frequency power supply adds rotating cathode and sputters at while carrying out in argon nitrogen atmosphere, and power is 30～40kw; Wherein, intermediate frequency power supply adds rotating cathode and sputters at while carrying out in argon oxygen atmosphere, and power is 30～50kw; It is to carry out in argon atmosphere or argon oxygen atmosphere that direct supply adds pulse sputter, and power is 0.6～3kw.
This silver-containing low emissivity glass increases silver layer, blocking layer and dielectric layer combination layer at traditional silver of take in the low emissivity glass of infrared external reflection rete, make like this silver thickness disperse and be blocked by the carrying of dielectric layer combination layer, when increasing silver thickness, visible light transmissivity is high, and outward appearance does not present interference color.
[accompanying drawing explanation]
Fig. 1 is the silver-containing low emissivity glass structural representation of an embodiment;
Fig. 2 is the manufacturing flow chart of the silver-containing low emissivity glass of an embodiment.
[embodiment]
A kind of silver-containing low emissivity glass as shown in Figure 1, comprises the following structure being arranged in order: glass substrate, basic unit's dielectric combination layer, the first silver layer, the first blocking layer, the first interlayer dielectric combination layer, the second silver layer, the second blocking layer, the second interlayer dielectric combination layer, the 3rd silver layer, the 3rd blocking layer, the 3rd interlayer dielectric combination layer, the 4th silver layer, the 4th blocking layer, upper strata dielectric combination layer.
Preferably, basic unit's dielectric combination layer, the first interlayer dielectric combination layer, the second interlayer dielectric combination layer, the 3rd interlayer dielectric combination layer, upper strata dielectric combination layer are by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations; The first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th blocking layer are by Ni, Cr, NiCrO
xand NiCrN
xin one or more formations.
Preferably, basic unit's dielectric combination layer thickness is 25～27nm; The first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th barrier layer thickness are 0.25～0.3nm; The first interlayer dielectric combination layer thickness is 67～69nm; The second interlayer dielectric combination layer thickness is 69～71nm; The 3rd interlayer dielectric combination layer thickness is 71～73nm; Upper strata dielectric combination layer thickness is 24～27nm.
Preferably, in four silver thickness, require the first silver thickness to be less than that the second silver layer, the second silver thickness are less than the 3rd silver layer, the 3rd silver thickness is less than the 4th silver layer.Four layers of silver thickness summation are about between 43nm～47nm, and its each silver thickness relation meets product appearance color as the color value scope in following table:
| Monolithic appearance color | Glass surface reflected colour | Rete face reflected colour | Transmitted colour |
| Y | Be less than 7 | Be less than 8 | Be greater than 70 |
| L* | Be less than 32 | Be less than 34 | Be greater than 87 |
| a* | -0.5～-1.8 | 1.2～1.8 | -6.0～-5.0 |
| b* | -3.5～-4.5 | -4.5～-5.5 | -1.0～2.0 |
Preferred, the first silver thickness is 7～8nm; The second silver thickness is 11～12nm; The 3rd silver thickness is 12～13nm; The 4th silver thickness is 13～14nm.
Preferably, upper strata dielectric combination layer comprises the first upper strata dielectric combination layer being deposited on the 4th blocking layer and is deposited on the second upper strata dielectric combination layer in the first upper strata dielectric combination layer; The first upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations; The second upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations; The thickness of the first upper strata dielectric combination layer is 15～16nm; The thickness of the second upper strata dielectric combination layer is 9～11nm.
Preferred, first, second upper strata dielectric combination layer forms with the stack of differing materials alternating sputtering conventionally, is convenient to control membrane uniformity, stability and reasonable optical effect.
Particularly preferred, the second upper strata dielectric combination layer outermost material at least comprises TiO
2, SiO
2and Si
3n
4in a kind of, make the wear-resisting and weather resistance of product finally meet physicochemical property standard.
The first upper strata dielectric combination layer thickness is about 1.5 times of the second upper strata dielectric combination layer thickness, makes product can obtain heat-resisting, durable and optics thermal characteristics relatively preferably.
The manufacture method of above-mentioned silver-containing low emissivity glass as shown in Figure 2, comprises the step that deposits successively each rete, specific as follows:
Clean glass substrate, the dry magnetron sputtering area that is placed on;
Intermediate frequency power supply adds rotating cathode sputtering sedimentation basic unit dielectric combination layer;
Direct supply adds pulse sputtering sedimentation the first silver layer;
Direct supply adds pulse sputtering sedimentation the first blocking layer;
Intermediate frequency power supply adds rotating cathode sputtering sedimentation the first interlayer dielectric combination layer;
Direct supply adds pulse sputtering sedimentation the second silver layer;
Direct supply adds pulse sputtering sedimentation the second blocking layer;
Intermediate frequency power supply adds rotating cathode sputtering sedimentation the second interlayer dielectric combination layer;
Direct supply adds pulse sputtering sedimentation the 3rd silver layer;
Direct supply adds pulse sputtering sedimentation the 3rd blocking layer;
Intermediate frequency power supply adds rotating cathode sputtering sedimentation the 3rd interlayer dielectric combination layer;
Direct supply adds pulse sputtering sedimentation the 4th silver layer;
Direct supply adds pulse sputtering sedimentation the 4th blocking layer;
Intermediate frequency power supply adds rotating cathode sputtering sedimentation upper strata dielectric combination layer;
Inspection after construction.
Preferably, during deposition plating, coating wire configuration keeping system background vacuum vacuum tightness is 3 * 10
-6dry molecular pump more than mbar; The contiguous compartment position of silver target disposes for absorbing the cryopump of moisture; It is to carry out in the argon nitrogen atmosphere that is 30～50kw at plant capacity or argon oxygen atmosphere that intermediate frequency power supply adds rotating cathode sputter, and frequency is 40kHz; Wherein, intermediate frequency power supply adds rotating cathode and sputters at while carrying out in argon nitrogen atmosphere, and power is 30～40kw; Wherein, intermediate frequency power supply adds rotating cathode and sputters at while carrying out in argon oxygen atmosphere, and power is 30～50kw; It is to carry out in argon atmosphere or argon oxygen atmosphere that direct supply adds pulse sputter, and power is 0.6～3kw;
Wherein, intermediate frequency power supply adds when rotating cathode sputtering sedimentation forms oxide skin and carries out in argon oxygen atmosphere, and in argon nitrogen atmosphere, carries out during formation of deposits nitride layer;
Direct supply adds when pulse sputtering sedimentation forms metal level or alloy layer and carries out in argon atmosphere, and in argon oxygen atmosphere, carries out during formation of deposits oxide skin.
The preparation of silver-containing low emissivity glass adopts vacuum magnetron sputtering coating film, and each rete can be by one matter formation of deposits, also can be by several different materials successively formation of deposits.
Below in conjunction with specific embodiment, silver-containing low emissivity glass and manufacture method thereof are further described.
Embodiment 1
The film layer structure of this silver-containing low emissivity glass embodiment 1 is followed successively by: glass, ZnSnO
x, Ag, NiCrO
x, ZnSnO
x, Ag, NiCrO
x, ZnSnO
x, Ag, NiCrO
x, ZnSnO
x, Ag, NiCrO
x, ZnSnO
x, Si
3n
4.
In the present embodiment, basic unit's dielectric combination layer is ZnSnO
xlayer, thickness is 27nm.
In the present embodiment, the first silver thickness is 8nm.
In the present embodiment, the first blocking layer is NiCrO
xlayer, thickness is 0.3nm.
In the present embodiment, the first interlayer dielectric combination layer layer is ZnSnO
xlayer, thickness is 69nm.
In the present embodiment, the second silver thickness is 12nm.
In the present embodiment, the second blocking layer is NiCrO
xlayer, thickness is 0.3nm.
In the present embodiment, the second interlayer dielectric combination layer layer is ZnSnO
xlayer, thickness is 71nm.
In the present embodiment, the 3rd silver thickness is 13nm.
In the present embodiment, the 3rd blocking layer is NiCrO
xlayer, thickness is 0.3nm.
In the present embodiment, the 3rd interlayer dielectric combination layer layer is ZnSnO
xlayer, thickness is 73nm.
In the present embodiment, the 4th silver thickness is 14nm.
In the present embodiment, the 4th blocking layer is NiCrO
xlayer, thickness is 0.3nm.
In the present embodiment, upper strata dielectric combination layer is by two kinds of compounds successively formation of deposits the first upper strata dielectric combination layer and the second upper strata dielectric combination layer; Wherein, the first upper strata dielectric combination layer is ZnSnO
xlayer, thickness is 16nm, the second upper strata dielectric combination layer is Si
3n
4layer, thickness is 11nm.
The concrete manufacturing process of above-mentioned each rete is:
Si
3n
4layer adopts intermediate frequency power supply to add rotating cathode and sputters at formation of deposits in argon nitrogen atmosphere, and vacuum magnetic-control sputtering plant capacity is 30～40kw, and intermediate frequency power supply frequency is 40kHz.
ZnSnO
xlayer adopts intermediate frequency power supply to add rotating cathode and sputters at formation of deposits in argon oxygen atmosphere, and vacuum magnetic-control sputtering plant capacity is 30～50kw, and intermediate frequency power supply frequency is 40kHz.
NiCrO
xlayer employing direct supply adds pulse and sputters at formation of deposits in argon oxygen atmosphere, and vacuum magnetic-control sputtering plant capacity is 0.6kw, argon flow amount 1000sccm, oxygen flux control is relevant with actual sputtering power, normally 10 multiple value of performance number, are 6sccm here, and object is in order to control NiCrO
xthe insufficient oxidation price of layer, the blocking capability that outstanding rete is stronger.
Ag layer adopts direct supply to add pulse and sputters at formation of deposits in argon atmosphere, and vacuum magnetic-control sputtering plant capacity is 3kw.
This silver-containing low emissivity glass optical property and thermal characteristics are as follows:
Radiant ratio ε≤0.02, (structure is hollow product: heat transfer coefficient U-value < 1.1W/m 6mm silver-containing low emissivity glass+12mm gas cloud+6mm common white glass)
2k, selects coefficient Lsg>=2.4.
With traditional low emissivity glass comparison containing three silver layers, this product radiant ratio is lower by 0.015 than three-silver low radiation glass, and (structure is ratio of heat transfer coefficient three-silver low radiation glass hollow product: 6mm three-silver low radiation glass+12mm gas cloud+6mm common white glass) low 0.3W/m
2k.
Four silver layers keep strict thickness, and this four silver-layer low-radiation glass appearance color meets:
| Monolithic appearance color | Glass surface reflected colour | Rete face reflected colour | Transmitted colour |
| Y | Be less than 7 | Be less than 8 | Be greater than 70 |
| L* | Be less than 32 | Be less than 34 | Be greater than 87 |
| a* | -0.5～-1.8 | 1.2～1.8 | -6.0～-5.0 |
| b* | -3.5～-4.5 | -4.5～-5.5 | -1.0～2.0 |
Embodiment 2
The film layer structure of another specific embodiment of this silver-containing low emissivity glass is followed successively by: glass, Si
3n
4, Ag, NiCr, Si
3n
4, Ag, NiCr, Si
3n
4, Ag, NiCr, Si
3n
4, Ag, NiCr, Si
3n
4, TiO
2.
In the present embodiment, basic unit's dielectric combination layer is Si
3n
4layer, thickness is 25nm.
In the present embodiment, the first silver thickness is 7.6nm.
In the present embodiment, the first blocking layer is NiCr layer, and thickness is 0.3nm.
In the present embodiment, the first interlayer dielectric combination layer layer is Si
3n
4layer, thickness is 67nm.
In the present embodiment, the second silver thickness is 10.8nm.
In the present embodiment, the second blocking layer is NiCr layer, and thickness is 0.3nm.
In the present embodiment, the second interlayer dielectric combination layer layer is Si
3n
4layer, thickness is 69nm.
In the present embodiment, the 3rd silver thickness is 13.3nm.
In the present embodiment, the 3rd blocking layer is NiCr layer, and thickness is 0.3nm.
In the present embodiment, the 3rd interlayer dielectric combination layer layer is Si
3n
4layer, thickness is 71nm.
In the present embodiment, the 4th silver thickness is 14nm.
In the present embodiment, the 4th blocking layer is NiCr layer, and thickness is 0.3nm.
In the present embodiment, upper strata dielectric combination layer is by two kinds of compounds successively formation of deposits the first upper strata dielectric combination layer and the second upper strata dielectric combination layer; Wherein, the first upper strata dielectric combination layer is Si
3n
4layer, thickness is 15nm, the second upper strata dielectric combination layer is TiO
2layer, thickness is 10nm.
The concrete manufacturing process of above-mentioned each rete is:
Si
3n
4layer adopts intermediate frequency power supply to add rotating cathode and sputters at formation of deposits in argon nitrogen atmosphere, and vacuum magnetic-control sputtering plant capacity is 30～40kw, and intermediate frequency power supply frequency is 40kHz.
TiO
2layer adopts intermediate frequency power supply to add rotating cathode and sputters at formation of deposits in argon nitrogen atmosphere, and vacuum magnetic-control sputtering plant capacity is 30～40kw, and intermediate frequency power supply frequency is 40kHz.
NiCr layer adopts direct supply to add pulse and sputters at formation of deposits in argon atmosphere, and vacuum magnetic-control sputtering plant capacity is 0.6kw, argon flow amount 1000sccm.
Ag layer adopts direct supply to add pulse and sputters at formation of deposits in argon atmosphere, and vacuum magnetic-control sputtering plant capacity is 3kw.
This silver-containing low emissivity glass optical property and thermal characteristics are as follows:
Radiant ratio ε≤0.02, (structure is hollow product: heat transfer coefficient U-value < 1.1W/m 6mm silver-containing low emissivity glass+12mm gas cloud+6mm common white glass)
2k, selects coefficient Lsg>=2.4.
With traditional low emissivity glass comparison containing three silver layers, this product radiant ratio is lower by 0.015 than three-silver low radiation glass, and (structure is ratio of heat transfer coefficient three-silver low radiation glass hollow product: 6mm three-silver low radiation glass+12mm gas cloud+6mm common white glass) low 0.3W/m
2k.
Four silver layers keep strict thickness, and this four silver-layer low-radiation glass appearance color meets:
| Monolithic appearance color | Glass surface reflected colour | Rete face reflected colour | Transmitted colour |
| Y | Be less than 7 | Be less than 8 | Be greater than 70 |
| L* | Be less than 32 | Be less than 34 | Be greater than 87 |
| a* | -0.5～-1.8 | 1.2～1.8 | -6.0～-5.0 |
| b* | -3.5～-4.5 | -4.5～-5.5 | -1.0～2.0 |
This silver-containing low emissivity glass increases silver layer, blocking layer and dielectric layer combination layer at traditional silver of take in the low emissivity glass of infrared external reflection rete, make like this silver thickness disperse and be blocked by the carrying of dielectric layer combination layer, when increasing silver thickness, visible light transmissivity is high, and outward appearance does not present interference color.
By rete, design, the blocking layer on silver layer both sides and dielectric combination layer thickness are maintained in certain proportional range, silver layer is had to the ability of better blocking; By coating process, make the blocking layer on silver layer and both sides thinner finer and close in addition.Like this, when keeping low radiation, effectively improve selection coefficient, obtained good overall target; Four silver layers keep strict thickness, and this four silver-layer low-radiation glass appearance color is met:
| Monolithic appearance color | Glass surface reflected colour | Rete face reflected colour | Transmitted colour |
| Y | Be less than 7 | Be less than 8 | Be greater than 70 |
| L* | Be less than 32 | Be less than 34 | Be greater than 87 |
| a* | -0.5～-1.8 | 1.2～1.8 | -6.0～-5.0 |
| b* | -3.5～-4.5 | -4.5～-5.5 | -1.0～2.0 |
Make like this this silver-containing low emissivity glass outward appearance better, select coefficient higher.
First, second upper strata dielectric combination layer forms with the stack of differing materials alternating sputtering conventionally, is convenient to control membrane uniformity, stability and reasonable optical effect.
The second upper strata dielectric combination layer outermost material at least comprises TiO
2, SiO
2and Si
3n
4in a kind of, make the wear-resisting and weather resistance of product finally meet physicochemical property standard.
The first upper strata dielectric combination layer thickness is about 1.5 times of the second upper strata dielectric combination layer thickness, makes product can obtain heat-resisting, durable and optics thermal characteristics relatively preferably.
During plated film, on coating wire, dispose the dry molecular pump of high pumping rate, keep background vacuum in high vacuum 3 * 10
-6more than mbar, system has good gas isolating effect between several processing atmospheres sputtering zone, isolating coefficient is greater than 30, there is good film uniformity and rete simultaneously and form homogeneity of ingredients, under the vacuum acquiring system of large pumping speed, strengthen the pressure of process gas, the cathode power that adopts direct current to add pulse carries out sputter, and absorb moisture at the contiguous compartment position of silver-colored target configuration cryopump, and improved the quality of forming film of silver layer, effectively raise the visible light transmissivity of product.
Basic unit's dielectric combination layer and interlayer dielectric combination layer are antireflection film layer, play a part to connect glass and functional layer, and between glass, adhesiveproperties are good simultaneously, and have alleviated the internal stress of whole low-radiation film.Upper strata dielectric combination layer has directly increased described silver-containing low emissivity glass scratch resistance, wear-resisting and erosion-resisting performance.The intermediate frequency power supply with good arc extinction performance of these two kinds of combination layer proportion 40kHz adds rotating cathode sputter and forms, and specific refractory power matched well, makes the reflectivity of product and transmitance reach ideal value.
This silver-containing low emissivity glass radiation is low, visible light transmissivity is high, outward appearance does not present interference color, select coefficient high, has good energy-saving effect; Unique film layer structure, makes product have good weathering resistance, simultaneously rete difficult drop-off, be difficult for oxidizedly, can be generalized to vehicle glass and residential houses.
The above embodiment has only expressed embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a silver-containing low emissivity glass, it is characterized in that, this glass film layer structure is followed successively by: glass substrate, basic unit's dielectric combination layer, the first silver layer, the first blocking layer, the first interlayer dielectric combination layer, the second silver layer, the second blocking layer, the second interlayer dielectric combination layer, the 3rd silver layer, the 3rd blocking layer, the 3rd interlayer dielectric combination layer, the 4th silver layer, the 4th blocking layer, upper strata dielectric combination layer;
In four silver thickness, require the first silver thickness to be less than that the second silver layer, the second silver thickness are less than the 3rd silver layer, the 3rd silver thickness is less than the 4th silver layer; Four layers of silver thickness summation are 43nm～47nm, and its each silver thickness relation meets product appearance color as the color value scope in following table:
；
Described upper strata dielectric combination layer comprises the first upper strata dielectric combination layer being deposited on described the 4th blocking layer and is deposited on the second upper strata dielectric combination layer in described the first upper strata dielectric combination layer;
The thickness of described the first upper strata dielectric combination layer is 15～16nm;
The thickness of described the second upper strata dielectric combination layer is 9～11nm;
Described the first upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations;
Described the second upper strata dielectric combination layer is by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more form, and at least comprise TiO
2, SiO
2and Si
3n
4in a kind of;
First, second upper strata dielectric combination layer forms with the stack of differing materials alternating sputtering;
The first upper strata dielectric combination layer thickness is 1.5 times of the second upper strata dielectric combination layer thickness.
2. silver-containing low emissivity glass as claimed in claim 1, is characterized in that, described basic unit dielectric combination layer, the first interlayer dielectric combination layer, the second interlayer dielectric combination layer, the 3rd interlayer dielectric combination layer are by TiO
2, ZnSnO
x, SnO
2, ZnO, SiO
2, Ta
2o
5, Bi
2o
3, Al
2o
3, ZnAl
2o
4, Nb
2o
5and Si
3n
4in one or more formations;
Described the first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th blocking layer are by Ni, Cr, NiCrO
xand NiCrN
xin one or more formations.
3. silver-containing low emissivity glass as claimed in claim 1, is characterized in that, described basic unit dielectric combination layer thickness is 25～27nm;
Described the first interlayer dielectric combination layer thickness is 67～69nm;
Described the second interlayer dielectric combination layer thickness is 69～71nm;
Described the 3rd interlayer dielectric combination layer thickness is 71～73nm;
Described upper strata dielectric combination layer thickness is 24～27nm.
4. silver-containing low emissivity glass as claimed in claim 1, is characterized in that, described the first blocking layer, the second blocking layer, the 3rd blocking layer, the 4th barrier layer thickness are 0.25～0.3nm.
5. silver-containing low emissivity glass as claimed in claim 1, is characterized in that, described the first silver thickness is 7～8nm; The second silver thickness is 11～12nm; The 3rd silver thickness is 12～13nm; The 4th silver thickness is 13～14nm.
6. a manufacture method for the silver-containing low emissivity glass as described in claim 1～5 any one, is characterized in that, comprises the step that deposits successively each rete, specific as follows:
S1, cleaning glass substrate, the dry magnetron sputtering area that is placed on;
S2, intermediate frequency power supply add rotating cathode sputtering sedimentation basic unit dielectric combination layer;
S3, direct supply add pulse sputtering sedimentation the first silver layer;
S4, direct supply add pulse sputtering sedimentation the first blocking layer;
S5, intermediate frequency power supply add rotating cathode sputtering sedimentation the first interlayer dielectric combination layer;
S6, direct supply add pulse sputtering sedimentation the second silver layer;
S7, direct supply add pulse sputtering sedimentation the second blocking layer;
S8, intermediate frequency power supply add rotating cathode sputtering sedimentation the second interlayer dielectric combination layer;
S9, direct supply add pulse sputtering sedimentation the 3rd silver layer;
S10, direct supply add pulse sputtering sedimentation the 3rd blocking layer;
S11, intermediate frequency power supply add rotating cathode sputtering sedimentation the 3rd interlayer dielectric combination layer;
S12, direct supply add pulse sputtering sedimentation the 4th silver layer;
S13, direct supply add pulse sputtering sedimentation the 4th blocking layer;
S14, intermediate frequency power supply add rotating cathode sputtering sedimentation upper strata dielectric combination layer.
7. the manufacture method of silver-containing low emissivity glass as claimed in claim 6, is characterized in that, during deposition plating, coating wire disposes the vacuum tightness of keeping system background vacuum 3 * 10
-6dry molecular pump more than mbar;
The contiguous compartment position of silver target disposes for absorbing the cryopump of moisture.
8. the manufacture method of silver-containing low emissivity glass as claimed in claim 6, is characterized in that, it is to carry out in argon nitrogen or argon oxygen atmosphere that described intermediate frequency power supply adds rotating cathode sputter, and frequency is 40kHz, and power is 30～50kw;
It is to carry out in argon atmosphere or argon oxygen atmosphere that described direct supply adds pulse sputter, and power is 0.6～3kw.
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| CN102584034A (en) * | 2012-03-19 | 2012-07-18 | 山东力诺新材料有限公司 | Low emissivity film for solar high temperature collector tube and forming process for low emissivity film |
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| CN104309217A (en) * | 2014-10-30 | 2015-01-28 | 中山市亨立达机械有限公司 | Double-silver-layer LOW-E (Low-emissivity) glass with simple structure |
| US10345499B2 (en) * | 2015-02-03 | 2019-07-09 | Vitro Flat Glass LLC.. | Solar control coating with enhanced solar control performance |
| CN105152549A (en) * | 2015-05-26 | 2015-12-16 | 信义玻璃工程（东莞）有限公司 | Coated glass and preparation method thereof |
| GB201820002D0 (en) | 2018-12-07 | 2019-01-23 | Pilkington Group Ltd | Coated glass pane |
| CN109734332B (en) * | 2019-01-26 | 2019-11-29 | 乐清市芮易经济信息咨询有限公司 | A kind of low radiation coated glass and its processing technology |
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