CN103614696A - Preparation method of corrosion-resistant thin film - Google Patents

Preparation method of corrosion-resistant thin film Download PDF

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Publication number
CN103614696A
CN103614696A CN201310552861.6A CN201310552861A CN103614696A CN 103614696 A CN103614696 A CN 103614696A CN 201310552861 A CN201310552861 A CN 201310552861A CN 103614696 A CN103614696 A CN 103614696A
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layer
sputtering
argon gas
preparation
magnetron sputtering
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CN103614696B (en
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陈路玉
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ZHONGSHAN GUANGWEI OPTOELECTRONIC TECHNOLOGY CO LTD
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Zhongshan Chuangke Scientific Research Technology Services Co Ltd
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Abstract

The invention discloses a preparation method of a corrosion-resistant thin film. The preparation method comprises the following steps: A) performing magnetron sputtering of a Bi2O3 layer on a transparent heat-resistant base plate by a direct current power supply sputtering Bi planar target; B) performing magnetron sputtering of a TiOx layer on the Bi2O3 layer by an alternating current power supply sputtering titanium oxide ceramic rotating target; C) performing magnetron sputtering of a CrNx layer on the TiOx layer by a direct current power supply sputtering chromium planar target; D) performing magnetron sputtering of a Cu layer on the CrNx layer by a direct current power supply sputtering copper planar target; E) performing magnetron sputtering of a NiCr layer on the Cu layer by a direct current power supply sputtering NiCr alloy planar target; and F) performing magnetron sputtering of a ZnSnO3 layer on the NiCr layer by an alternating current power supply sputtering ZnSn alloy rotating target. The invention aims at overcoming the shortcomings in the prior art and providing the preparation method of the corrosion-resistant thin film, which has the advantages of simple process, convenience in operation and relatively low production cost.

Description

A kind of preparation method of etching resistant film
Technical field
The present invention relates to a kind of preparation method of etching resistant film.
Background technology
Low emissivity glass refers to that ir radiation is had to high-reflectivity, 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.
More common low emissivity glass 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. in the market.Existing these four kinds of low emissivity glasses are not high enough in the visible wavelength range internal transmission factor of 380~780 nanometers, are only 50% left and right; Higher in ir radiation wavelength region internal transmission factor, especially the wavelength region internal transmission factor in 900~1100 nanometers is between 10~20%.In addition, the wear resistance of these glass is conventionally good not.
And the rotproofness of existing transparent substrate is relative with thermotolerance poor, so existing transparent substrate awaits progressive perfect.
Summary of the invention
The object of the invention is, in order to overcome weak point of the prior art, provides a kind of technique simple, easy to operate, the preparation method of the etching resistant film that production cost is relatively low.
In order to achieve the above object, the present invention adopts following scheme:
A preparation method for etching resistant film, is characterized in that comprising the following steps:
A, adopt oxygen as reactant gases, argon gas is as shielding gas, direct supply sputter Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate 2o 3layer;
B, adopt argon gas as reactant gases, AC power sputter titanium oxide ceramics rotary target, Bi in steps A 2o 3magnetron sputtering TiO on layer xlayer;
C, adopt nitrogen as reactant gases, argon gas is as shielding gas, direct supply sputter chromium planar target, the TiO in step B xmagnetron sputtering C rN on layer xlayer;
D, adopt argon gas as reactant gases, direct supply sputter copper planar target, the CrN in step C xmagnetron sputtering C u layer on layer;
E, adopt argon gas as reactant gases, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on the Cu layer in step D;
F, adopt oxygen as reactant gases, argon gas is as shielding gas, AC power sputter ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e 3layer.
The preparation method of a kind of etching resistant film as above, is characterized in that Bi described in steps A 2o 3the thickness of layer is 10~15nm, and the volume ratio of oxygen and argon gas is 1:2, and the sputtering power of described direct supply is 15~20KW.
The preparation method of a kind of etching resistant film as above, is characterized in that TiO described in step B xthe thickness of layer is 10~15nm, the sputtering power 50~75KW of described AC power.
The preparation method of a kind of etching resistant film as above, is characterized in that CrN described in step C xthe thickness of layer is 3~5nm, and the volume ratio of described nitrogen and argon gas is 1:2, the sputtering power 3~6KW of described direct supply.
The preparation method of a kind of etching resistant film as above, is characterized in that the thickness of Cu layer is 10~20nm described in step D, the sputtering power 3~6KW of described direct supply.
The preparation method of a kind of etching resistant film as above, the thickness that it is characterized in that the layer of NiCr described in step e is 3~5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3~5KW of described direct supply.
The preparation method of a kind of etching resistant film as above, is characterized in that ZnSnO described in F 3the thickness of layer is 20~30nm, the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, and the volume ratio of described argon gas and oxygen is 1:2, the sputtering power of described AC power is 50~75KW.
The preparation method of a kind of etching resistant film as above, is characterized in that transparency and heat-proof substrate is transparent glass.
In sum, beneficial effect of the present invention:
Processing method of the present invention is simple, easy to operate, and production cost is relatively low.Product erosion resistance is strong, less demanding to substrate clean level in production process, product transmittance T >=65% of the present invention, radiant ratio E≤0.15.
Embodiment
Below in conjunction with embodiment, the present invention is described further:
Embodiment 1
The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:
A, adopt oxygen as reactant gases, argon gas is as shielding gas, direct supply sputter Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate 2o 3layer; Wherein said Bi 2o 3the thickness of layer is 10nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm, and the sputtering power of described direct supply is 15KW, and wherein said transparency and heat-proof substrate is transparent glass;
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputter titanium oxide ceramics rotary target, Bi in steps A 2o 3magnetron sputtering TiO on layer xlayer; Wherein said TiO xthe thickness of layer is 10nm, the sputtering power 50KW of described AC power;
C, adopt nitrogen as reactant gases, argon gas is as shielding gas, direct supply sputter chromium planar target, the TiO in step B xmagnetron sputtering C rN on layer xlayer; Wherein said CrN xthe thickness of layer is 3nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 3KW of described direct supply;
D, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm direct supply sputter copper planar target, the CrN in step C xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 10nm, 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 the Cu layer in step D; 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;
F, adopt oxygen as reactant gases, argon gas is as shielding gas, AC power sputter ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e 3layer; Described ZnSnO 3the thickness of layer is 20nm, the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, and the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, the sputtering power of described AC power is 50KW.
Embodiment 2
The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:
A, adopt oxygen as reactant gases, argon gas is as shielding gas, direct supply sputter Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate 2o 3layer; Wherein said Bi 2o 3the thickness of layer is 12nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm,, the sputtering power of described direct supply is 18KW, wherein said transparency and heat-proof substrate is transparent glass;
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputter titanium oxide ceramics rotary target, Bi in steps A 2o 3magnetron sputtering TiO on layer xlayer; Wherein said TiO xthe thickness of layer is 13nm, the sputtering power 60KW of described AC power;
C, adopt nitrogen as reactant gases, argon gas is as shielding gas, direct supply sputter chromium planar target, the TiO in step B xmagnetron sputtering C rN on layer xlayer; Wherein said CrN xthe thickness of layer is 4nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 5KW of described direct supply;
D, adopt argon gas as reactant gases, direct supply sputter copper planar target, the CrN in step C xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 15nm, the sputtering power 4KW 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 the Cu layer in step D; The thickness of described NiCr layer is 4nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 4KW of described direct supply;
F, adopt oxygen as reactant gases, argon gas is as shielding gas, AC power sputter ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e 3layer.Described ZnSnO 3the thickness of layer is 25nm, the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, and the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, the sputtering power of described AC power is 63KW.
Embodiment 3
The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:
A, adopt oxygen as reactant gases, argon gas is as shielding gas, direct supply sputter Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate 2o 3layer; Wherein said Bi 2o 3the thickness of layer is 15nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm,, the sputtering power of described direct supply is 20KW, wherein said transparency and heat-proof substrate is transparent glass;
B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputter titanium oxide ceramics rotary target, Bi in steps A 2o 3magnetron sputtering TiO on layer xlayer; Wherein said TiO xthe thickness of layer is 15nm, the sputtering power 75KW of described AC power;
C, adopt nitrogen as reactant gases, argon gas is as shielding gas, direct supply sputter chromium planar target, the TiO in step B xmagnetron sputtering C rN on layer xlayer; Wherein said CrN xthe thickness of layer is 5nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 6KW of described direct supply;
D, adopt argon gas as reactant gases, direct supply sputter copper planar target, the CrN in step C xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 20nm, the sputtering power 6KW 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 the Cu layer in step D; The thickness of described NiCr layer is 5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 5KW of described direct supply;
F, adopt oxygen as reactant gases, argon gas is as shielding gas, AC power sputter ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e 3layer.Described ZnSnO 3the thickness of layer is 30nm, the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, and the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, the sputtering power of described AC power is 75KW.
More than show and described 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; that in above-described embodiment and specification sheets, describes 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.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (8)

1. a preparation method for etching resistant film, is characterized in that comprising the following steps:
A, adopt oxygen as reactant gases, argon gas is as shielding gas, direct supply sputter Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate 2o 3layer;
B, adopt argon gas as reactant gases, AC power sputter titanium oxide ceramics rotary target, Bi in steps A 2o 3magnetron sputtering TiO on layer xlayer;
C, adopt nitrogen as reactant gases, argon gas is as shielding gas, direct supply sputter chromium planar target, the TiO in step B xmagnetron sputtering C rN on layer xlayer;
D, adopt argon gas as reactant gases, direct supply sputter copper planar target, the CrN in step C xmagnetron sputtering C u layer on layer;
E, adopt argon gas as reactant gases, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on the Cu layer in step D;
F, adopt oxygen as reactant gases, argon gas is as shielding gas, AC power sputter ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e 3layer.
2. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that Bi described in steps A 2o 3the thickness of layer is 10~15nm, and the volume ratio of oxygen and argon gas is 1:2, and the sputtering power of described direct supply is 15~20KW.
3. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that TiO described in step B xthe thickness of layer is 10~15nm, the sputtering power 50~75KW of described AC power.
4. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that CrN described in step C xthe thickness of layer is 3~5nm, and the volume ratio of described nitrogen and argon gas is 1:2, the sputtering power 3~6KW of described direct supply.
5. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that the thickness of Cu layer is 10~20nm described in step D, the sputtering power 3~6KW of described direct supply.
6. the preparation method of a kind of etching resistant film according to claim 1, the thickness that it is characterized in that the layer of NiCr described in step e is 3~5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3~5KW of described direct supply.
7. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that ZnSnO described in F 3the thickness of layer is 20~30nm, the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, and the volume ratio of described argon gas and oxygen is 1:2, the sputtering power of described AC power is 50~75KW.
8. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that transparency and heat-proof substrate is transparent glass.
CN201310552861.6A 2013-11-07 2013-11-07 A kind of preparation method of etching resistant film Active CN103614696B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107740061A (en) * 2017-10-27 2018-02-27 中山市汉庭照明科技有限公司 A kind of method for preparing corrosion-resistant Crystal lamp suspension member
CN107740975A (en) * 2017-10-27 2018-02-27 中山市汉庭照明科技有限公司 A kind of corrosion-resistant Crystal lamp suspension member
WO2021159680A1 (en) * 2020-08-17 2021-08-19 广东省科学院测试分析研究所(中国广州分析测试中心) Inverted heating method for preparing oxidized bismuth nanowire thin film
CN115928015A (en) * 2022-11-25 2023-04-07 广东省人民医院 Titanium surface modification method with osteogenesis promoting and immunoregulation performances

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Publication number Priority date Publication date Assignee Title
CN107740061A (en) * 2017-10-27 2018-02-27 中山市汉庭照明科技有限公司 A kind of method for preparing corrosion-resistant Crystal lamp suspension member
CN107740975A (en) * 2017-10-27 2018-02-27 中山市汉庭照明科技有限公司 A kind of corrosion-resistant Crystal lamp suspension member
WO2021159680A1 (en) * 2020-08-17 2021-08-19 广东省科学院测试分析研究所(中国广州分析测试中心) Inverted heating method for preparing oxidized bismuth nanowire thin film
CN115928015A (en) * 2022-11-25 2023-04-07 广东省人民医院 Titanium surface modification method with osteogenesis promoting and immunoregulation performances

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