CN103643208B - A kind of preparation method of high film - Google Patents
A kind of preparation method of high film Download PDFInfo
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- CN103643208B CN103643208B CN201310548946.7A CN201310548946A CN103643208B CN 103643208 B CN103643208 B CN 103643208B CN 201310548946 A CN201310548946 A CN 201310548946A CN 103643208 B CN103643208 B CN 103643208B
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Abstract
The invention discloses a kind of preparation method of high film, it is characterized in that comprising the following steps: A, direct supply sputtering Nb planar target, magnetron sputtering Nb on transparent heat-resistant glass substrate
2o
5layer; B, AC power sputtering titanium oxide ceramics rotary target, at Nb
2o
5magnetron sputtering TiO on layer
2layer; C, AC power sputtering Al-Doped ZnO ceramic target rotary target, at TiO
2magnetron sputtering AZO layer on layer; D, direct supply sputtering silver planar target, magnetron sputtering Ag layer on AZO layer; E, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer; F, AC power sputtering titanium oxide ceramics rotary target, magnetron sputtering TiO on NiCr layer
2layer.The object of the invention is to overcome weak point of the prior art, providing a kind of technique simple, easy to operate, the preparation method of the saturating film of height that production cost is relatively low.
Description
Technical field
The present invention relates to a kind of preparation method of high film.
Background technology
Low emissivity glass refers to have high-reflectivity to ir radiation, visible ray is had to the flat plate film coating glass of good transmissivity.Low emissivity glass has good printing opacity, insulation, heat-proof quality, is widely used in the places such as window, fire door, refrigerator door.
Low emissivity glass more common in the market has single silver-layer low-radiation glass, two silver-layer low-radiation glass, thermal control low emissivity glass and titanium base low emissivity glass etc.These four kinds of low emissivity glasses existing are not high enough in the visible wavelength range internal transmission factor of 380 ~ 780 nanometers, are only about 50%; Higher in infrared radiation wavelength scope internal transmission factor, be especially between 10 ~ 20% in the wavelength region internal transmission factor of 900 ~ 1100 nanometers.In addition, the wear resistance of these glass is usually excellent not.
So existing clear glass substrate awaits progressive perfect.
Summary of the invention
The object of the invention is to overcome weak point of the prior art, providing a kind of technique simple, easy to operate, the preparation method of the saturating film of height that production cost is relatively low.
In order to achieve the above object, the present invention adopts following scheme:
A preparation method for high film, is characterized in that comprising the following steps:
A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Nb planar target, magnetron sputtering Nb on transparent heat-resistant glass substrate
2o
5layer;
B, employing argon gas are as reactant gases, and AC power sputters titanium oxide ceramics rotary target, Nb in step
2o
5magnetron sputtering TiO on layer
2layer;
C, employing argon gas are as reactant gases, and AC power sputters Al-Doped ZnO ceramic target rotary target, TiO in stepb
2magnetron sputtering AZO layer on layer;
D, adopt argon gas as reactant gases, direct supply sputtering silver planar target, magnetron sputtering Ag layer on the AZO layer in step C;
E, adopt argon gas as reactant gases, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer in step D;
F, employing argon gas are as reactant gases, and AC power sputters titanium oxide ceramics rotary target, magnetron sputtering TiO on the NiCr layer in step e
2layer.
The preparation method of a kind of high film as above, is characterized in that Nb described in steps A
2o
5the thickness of layer is 20 ~ 30nm, and the volume ratio of argon gas and oxygen is 1:3, sputtering pressure 2.5*10
-3mbar, the sputtering power of described direct supply is 30 ~ 45KW.
The preparation method of a kind of high film as above, is characterized in that TiO described in step B
2the thickness of layer is 8 ~ 15nm, the sputtering power 40 ~ 75KW of described AC power.
The preparation method of a kind of high film as above, is characterized in that the thickness of the layer of AZO described in step C is 20 ~ 25nm, the sputtering power 20 ~ 25KW of described AC power.
The preparation method of a kind of high film as above, is characterized in that the thickness of Ag layer described in step D is 8 ~ 10nm, the sputtering power 3 ~ 6KW of described direct supply.
The preparation method of a kind of high film as above, is characterized in that the thickness of the layer of NiCr described in step e is 2 ~ 3nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 2 ~ 3KW of described direct supply.
The preparation method of a kind of high film as above, is characterized in that TiO described in F
2the thickness of layer is 20 ~ 30nm, and the sputtering power of described AC power is 100 ~ 150KW, comprising two cathode sputterings, and each negative electrode 50 ~ 75KW.
In sum, beneficial effect of the present invention:
Present invention process method is simple, and easy to operate, production cost is relatively low.Product transmitance up to more than 85%, close to substrate transmitance; Less demanding to substrate clean level in production process, mechanical property is excellent.
Embodiment
Below in conjunction with embodiment, the present invention is described further:
Embodiment 1
The preparation method of a kind of high film of the present invention, comprises the following steps:
A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Nb planar target, magnetron sputtering Nb on transparent heat-resistant glass substrate
2o
5layer; Described Nb
2o
5the thickness of layer is 20nm, and the volume ratio of argon gas and oxygen is 1:3, i.e. argon gas: oxygen=300sccm:900sccm, sputtering pressure 2.5*10
-3mbar, the sputtering power of described direct supply is 30KW.
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Nb in step
2o
5magnetron sputtering TiO on layer
2layer; Described TiO
2the thickness of layer is 8nm, the sputtering power 40KW of described AC power.
C, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, and AC power sputtering Al-Doped ZnO ceramic target rotary target, wherein zinc-oxide ceramic target rotary target mixes aluminium 2%, TiO in stepb
2magnetron sputtering AZO layer on layer; The thickness of described AZO layer is 20nm, the sputtering power 20KW of described AC power.
D, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering silver planar target, magnetron sputtering Ag layer on the AZO layer in step C; The thickness of described Ag layer is 8nm, the sputtering power 3KW of described direct supply.The thickness of described NiCr layer is 2nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 2KW of described direct supply.
E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer in step D;
F, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, magnetron sputtering TiO on the NiCr layer in step e
2layer.Described TiO
2the thickness of layer is 20nm, and the sputtering power of described AC power is 100KW, comprising two cathode sputterings, and each negative electrode 50KW.
Embodiment 2
The preparation method of a kind of high film of the present invention, comprises the following steps:
A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Nb planar target, magnetron sputtering Nb on transparent heat-resistant glass substrate
2o
5layer; Described Nb
2o
5the thickness of layer is 25nm, and the volume ratio of argon gas and oxygen is 1:3, i.e. argon gas: oxygen=300sccm:900sccm, sputtering pressure 2.5*10
-3mbar, the sputtering power of described direct supply is 40KW.
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Nb in step
2o
5magnetron sputtering TiO on layer
2layer; Described TiO
2the thickness of layer is 10nm, the sputtering power 58KW of described AC power.
C, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, and AC power sputtering Al-Doped ZnO ceramic target rotary target, wherein zinc-oxide ceramic target rotary target mixes aluminium 2%, TiO in stepb
2magnetron sputtering AZO layer on layer; The thickness of described AZO layer is 22nm, the sputtering power 23KW of described AC power.
D, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering silver planar target, magnetron sputtering Ag layer on the AZO layer in step C; The thickness of described Ag layer is 9nm, the sputtering power 3 ~ 6KW of described direct supply.The thickness of described NiCr layer is 2.5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 22.5KW of described direct supply.
E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer in step D;
F, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, magnetron sputtering TiO on the NiCr layer in step e
2layer.Described TiO
2the thickness of layer is 20 ~ 30nm, and the sputtering power of described AC power is 120KW, comprising two cathode sputterings, and each negative electrode 60KW.
Embodiment 3
The preparation method of a kind of high film of the present invention, comprises the following steps:
A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Nb planar target, magnetron sputtering Nb on transparent heat-resistant glass substrate
2o
5layer; Described Nb
2o
5the thickness of layer is 30nm, and the volume ratio of argon gas and oxygen is 1:3, i.e. argon gas: oxygen=300sccm:900sccm, sputtering pressure 2.5*10
-3mbar, the sputtering power of described direct supply is 45KW.
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Nb in step
2o
5magnetron sputtering TiO on layer
2layer; Described TiO
2the thickness of layer is 15nm, the sputtering power 75KW of described AC power.
C, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, and AC power sputtering Al-Doped ZnO ceramic target rotary target, wherein zinc-oxide ceramic target rotary target mixes aluminium 2%, TiO in stepb
2magnetron sputtering AZO layer on layer; The thickness of described AZO layer is 25nm, the sputtering power 25KW of described AC power.
D, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering silver planar target, magnetron sputtering Ag layer on the AZO layer in step C; The thickness of described Ag layer is 10nm, the sputtering power 6KW of described direct supply.The thickness of described NiCr layer is 3nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3KW of described direct supply.
E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer in step D;
F, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, magnetron sputtering TiO on the NiCr layer in step e
2layer.Described TiO
2the thickness of layer is 30nm, and the sputtering power of described AC power is 150KW, comprising two cathode sputterings, and each negative electrode 75KW.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. a preparation method for high film, is characterized in that comprising the following steps:
A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Nb planar target, magnetron sputtering Nb2O5 layer on transparent heat-resistant glass substrate;
B, employing argon gas are as reactant gases, and AC power sputters titanium oxide ceramics rotary target, magnetron sputtering TiO2 layer on Nb2O5 layer in step;
C, employing argon gas are as reactant gases, and AC power sputters Al-Doped ZnO ceramic target rotary target, magnetron sputtering AZO layer on TiO2 layer in stepb;
D, adopt argon gas as reactant gases, direct supply sputtering silver planar target, magnetron sputtering Ag layer on the AZO layer in step C;
E, adopt argon gas as reactant gases, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Ag layer in step D;
F, employing argon gas are as reactant gases, and AC power sputters titanium oxide ceramics rotary target, magnetron sputtering TiO2 layer on the NiCr layer in step e.
2. the preparation method of a kind of high film according to claim 1, it is characterized in that the thickness of the layer of Nb2O5 described in steps A is 20 ~ 30nm, the volume ratio of argon gas and oxygen is 1:3, sputtering pressure 2.5*10-3mbar, and the sputtering power of described direct supply is 30 ~ 45kW.
3. the preparation method of a kind of high film according to claim 1, is characterized in that the thickness of the layer of TiO2 described in step B is 8 ~ 15nm, the sputtering power 40 ~ 75kW of described AC power.
4. the preparation method of a kind of high film according to claim 1, is characterized in that the thickness of the layer of AZO described in step C is 20 ~ 25nm, the sputtering power 20 ~ 25kW of described AC power.
5. the preparation method of a kind of high film according to claim 1, is characterized in that the thickness of Ag layer described in step D is 8 ~ 10nm, the sputtering power 3 ~ 6kW of described direct supply.
6. the preparation method of a kind of high film according to claim 1, is characterized in that the thickness of the layer of NiCr described in step e is 2 ~ 3nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 2 ~ 3kW of described direct supply.
7. the preparation method of a kind of high film according to claim 1, is characterized in that the thickness of the layer of TiO2 described in F is 20 ~ 30nm, and the sputtering power of described AC power is 100 ~ 150kW, comprising two cathode sputterings, and each negative electrode 50 ~ 75kW.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310548946.7A CN103643208B (en) | 2013-11-07 | 2013-11-07 | A kind of preparation method of high film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310548946.7A CN103643208B (en) | 2013-11-07 | 2013-11-07 | A kind of preparation method of high film |
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| CN103643208A CN103643208A (en) | 2014-03-19 |
| CN103643208B true CN103643208B (en) | 2016-01-20 |
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|---|---|---|---|
| CN201310548946.7A Active CN103643208B (en) | 2013-11-07 | 2013-11-07 | A kind of preparation method of high film |
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| CN104817277B (en) * | 2015-04-21 | 2017-04-19 | 福建省诺希科技园发展有限公司 | Method for preparing radiation-proof glass by silver composite target and product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2701475B1 (en) * | 1993-02-11 | 1995-03-31 | Saint Gobain Vitrage Int | Glass substrates coated with a stack of thin layers, application to glazing with infrared reflection properties and / or properties in the field of solar radiation. |
| FR2784985B1 (en) * | 1998-10-22 | 2001-09-21 | Saint Gobain Vitrage | TRANSPARENT SUBSTRATE PROVIDED WITH A STACK OF THIN FILMS |
| CN1208274C (en) * | 2001-01-09 | 2005-06-29 | 上海耀华皮尔金顿玻璃股份有限公司 | Absorption-type low-radiation film coated glass |
| KR20140024416A (en) * | 2011-05-30 | 2014-02-28 | 아사히 가라스 가부시키가이샤 | Low emissivity laminate and multi-layer glass |
| CN202943942U (en) * | 2012-12-05 | 2013-05-22 | 金堆城洛阳节能玻璃有限公司 | High-transmittance type temperable low-emissivity coated glass |
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Effective date of registration: 20160607 Address after: 528400 Guangdong city of Zhongshan province Zhongshan city Kangle Torch Development Zone Road Venture Building, room 146 Patentee after: Zhongshan everything Culture Development Co., Ltd. Address before: 528400 Zhongshan Torch Development Zone, Guangdong Venture Building No. 229 Patentee before: Zhongshan Chuangke Scientific Research Technology Services Co., Ltd. |
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Effective date of registration: 20211221 Address after: 528400 zone B, floor 1, building a, No. 13, Jingye Road, Torch Development Zone, Zhongshan City, Guangdong Province Patentee after: ZHONGSHAN ZHONGWANG OPTICS Co.,Ltd. Address before: 528400 room 146, Chuangye building, Kangle Avenue, Torch Development Zone, Zhongshan City, Guangdong Province Patentee before: ZHONGSHAN WANWU CULTURE DEVELOPMENT CO.,LTD. |