CN101752026A - Infrared transparent conductive film and preparation method thereof - Google Patents
Infrared transparent conductive film and preparation method thereof Download PDFInfo
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- CN101752026A CN101752026A CN201010013649A CN201010013649A CN101752026A CN 101752026 A CN101752026 A CN 101752026A CN 201010013649 A CN201010013649 A CN 201010013649A CN 201010013649 A CN201010013649 A CN 201010013649A CN 101752026 A CN101752026 A CN 101752026A
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Abstract
The invention discloses an infrared transparent conductive film and a preparation method thereof. The infrared transparent conductive film is prepared by covering Cu film and CuAlO film on sapphire substrate in turn. The thickness of the Cu film is 300-360nm, the refractive index is 1.07-1.13; and the thickness of the CuAlO film is 100-170nm and the refractive index is 1.70-2.00. During preparation, the radio frequency magnetron sputtering method is used to deposit Cu film on sapphire substrate, then annealing is performed, then the radio frequency magnetron sputtering method is used again to deposit CuAlO film on the sapphire with Cu film and then the annealing is performed. The prepared infrared transparent conductive Cu/CuAlO film of the invention has good infrared transmitting performance and conductivity, and can be used for improving the optical property and anti-electromagnetic interference performance of the infrared detector window/hood material.
Description
Technical field
The present invention relates to material science, specifically is a kind of infrared transparent conductive film and preparation method thereof.
Background technology
At present, infrared acquisition and guidance technology almost have been applied to various military combat platforms.Infrared Detectors window/head-shield is separated infrared sensing/imaging system and external environment, and system is played protective effect.Detector window/the hood material that can be used as 3～5um medium wave infrared band has yittrium oxide, spinelle, nitrogen oxygen aluminium, sapphire etc.The demand for development Infrared Detectors window/hood material of modern military and space technology also will possess the performance of anti-electromagnetic interference except wanting to bear the bump of solids such as free dust in high temperature, high pressure, thermal shock, the atmosphere and hail.These Infrared Detectors window/hood material directly contact with ambient atmosphere, all have a common weakness, and that is exactly that the electromagnetic shielding efficiency of material itself is all very low, is easy to be subjected to electromagnetic interference.
Extraneous so on the one hand electromagnetic energy will produce electromagnetic interference to detection system, and the normal running of electronics and electrical system is caused all bad consequences, make equipment or system works malfunctioning.The electronic equipment of detection system itself can produce electromagnetic radiation and might become the clue that the enemy scouts on the other hand, thereby military target is exposed.For being implemented in the function that increases shielding electromagnetic wave on the original function basis that does not change optical system, can prepare one deck on detector window/head-shield can efficiently see through useful infrared light, simultaneously again can the electromagnetic transparent conductive film of high-efficiency shielding.Thereby can eliminate or reduce the electromagnetic interference of missile emplacements, improve the survival ability of position in future war, therefore the development of high-effect infrared transparent conductive film is significant with exploitation.
Canada air-sea tactical operations center adopts radio frequency magnetron sputtering method to prepare CuAlO film (L.F.Johnson, " Infrared Transparent Conductive Oxides " .Proc.SPIE.2001.Vol.4375.Window and Dome Technologies and Materials VII), and studied the infrared transmission performance of CuAlO film and electric conductivity variation relation M.B.Moran. with thin film composition.By regulating the composition of CuAlO film, the infrared transmission performance and the electric conductivity of change CuAlO film that can be suitable.But for the research of CuAlO film, have a difficult problem, promptly the infrared transmission performance of CuAlO film and electric conductivity can not reach best simultaneously.Thereby the researcher can select a compromise way usually, promptly designs the composition of CuAlO film, makes the infrared transmission performance of CuAlO film and electric conductivity all reach a medium level.The CuAlO film of preparing does not so have good infrared transmittivity, and does not have good effectiveness yet.Thereby, can not improve the optical property and the anti-electromagnetic interference performance of Infrared Detectors window/hood material significantly.
Summary of the invention
For infrared transmission performance and the electric conductivity that overcomes infrared transparent conductive film in the prior art can not reach best deficiency simultaneously, the present invention proposes a kind of infrared transparent conductive film Cu/CuAlO and preparation method thereof.
The technical scheme that the present invention takes is: be coated with Cu film and CuAlO film on Sapphire Substrate successively.The thickness of Cu film is 300～360nm, and refractive index is 1.07～1.13; The thickness of CuAlO film is 100～170nm, and refractive index is 1.70～2.00.
The present invention also proposes a kind of method for preparing infrared transparent conductive film Cu/CuAlO, may further comprise the steps:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of rf magnetron sputtering are: sputtering power is 70～90W, and the Ar throughput is 17.0～24.0SCCM, and underlayer temperature is 150～300 ℃, and target-substrate distance is 6.2～7.0cm, and sputtering pressure is 0.2～0.5Pa, sedimentation time 2.5～4.0h.
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 30～60W, and Al target sputtering power is 80～110W, and the Ar throughput is 12.0～20.0SCCM, O
2Throughput is 10.0～16.0SCCM, and underlayer temperature is 350～500 ℃, and target-substrate distance is 6.0～9.0cm, and sputtering pressure is 0.2～0.5Pa, and sedimentation time is 2.5～3.4h.
Step 4, the sapphire that the surface is deposited the CuAlO film carries out annealing in process; The process conditions of annealing in process are: annealing temperature is 450～600 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.4～0.6h.Obtain the Cu/CuAlO bilayer film.
The present invention deposits the Cu film as transition zone on Sapphire Substrate, and deposits the CuAlO film on the transition zone of Cu film.Because the Cu film has splendid electric conductivity, can reduce the resistivity and the square resistance of CuAlO film, thereby make the Cu/CuAlO film have excellent conducting performance.As can be seen from Figure 1, the square resistance of Cu/CuAlO film of the present invention after 450 ℃ of annealing is less, be about 200 Ω/ (the more little correspondence of the square resistance conductivity of film is big more, and promptly the electric conductivity of film is good more), illustrate that the Cu/CuAlO film has excellent conducting performance.In addition, as can be seen from Figure 2, the infrared transmittivity of plated film Sapphire Substrate is not lower, be coated with Cu/CuAlO film of the present invention on the Sapphire Substrate after its infrared transmittivity obviously improve, illustrate that the Cu/CuAlO film has good infrared transmission performance.This shows that the Cu/CuAlO film has excellent conducting performance and good infrared transmission performance, is a kind of infrared transparent conductive film with applications well prospect.
Description of drawings
Fig. 1 is 300nm for the thickness of Cu film, and refractive index is 1.07; The thickness of CuAlO film is 170nm, and refractive index is 1.70 o'clock, and the square resistance of Cu/CuAlO film is with the variation relation of annealing temperature;
Fig. 2 for before the same Sapphire Substrate plated film with the infrared transmission performance contrast that is coated with behind the Cu/CuAlO film;
Fig. 3 prepares the flow chart of infrared transparent conductive film Cu/CuAlO for the present invention.Wherein:
1. the sapphire before sapphire 2. plated films behind the plating Cu/CuAlO film
Embodiment
Embodiment one
The described technical scheme of present embodiment is to be coated with Cu film and CuAlO film on Sapphire Substrate successively.The thickness of Cu film is 300nm, and refractive index is 1.07; The thickness of CuAlO film is 170nm, and refractive index is 1.70.
The concrete preparation process of present embodiment is:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of deposition are: sputtering power is 90W, and the Ar throughput is 17.0SCCM, and underlayer temperature is 150 ℃, and target-substrate distance is 6.2cm, and sputtering pressure is 0.5Pa, and sedimentation time is 2.5h.
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 30W, and Al target sputtering power is 110W, and the Ar throughput is 12.0SCCM, O
2Throughput is 10.0SCCM, and underlayer temperature is 350 ℃, and target-substrate distance is 9.0cm, and sputtering pressure is 0.5Pa, and sedimentation time is 3.4h.
Step 4, the sapphire that the surface is deposited the CuAlO film carries out annealing in process; Process conditions are: annealing temperature is 450 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.6h.Obtain the Cu/CuAlO bilayer film.
Embodiment two
The described technical scheme of present embodiment is to be coated with Cu film and CuAlO film on Sapphire Substrate successively.The thickness of Cu film is 330nm, and refractive index is 1.10; The thickness of CuAlO film is 140nm, and refractive index is 1.80.
The concrete preparation process of present embodiment is:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of deposition are: sputtering power is 80W, and the Ar throughput is 19.0SCCM, and underlayer temperature is 200 ℃, and target-substrate distance is 6.5cm, and sputtering pressure is 0.4Pa, and sedimentation time is 3.0h.
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 40W, and Al target sputtering power is 100W, and the Ar throughput is 15.0SCCM, O
2Throughput is 12.0SCCM, and underlayer temperature is 400 ℃, and target-substrate distance is 8.0cm, and sputtering pressure is 0.4Pa, and sedimentation time is 3.0h.
Step 4, the sapphire that the surface is deposited the CuAlO film carries out annealing in process; The process conditions of annealing are: annealing temperature is 500 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.5h.Obtain the Cu/CuAlO bilayer film.
Embodiment three
The described technical scheme of present embodiment is to be coated with Cu film and CuAlO film on Sapphire Substrate successively.The thickness of Cu film is 360nm, and refractive index is 1.11; The thickness of CuAlO film is 110nm, and refractive index is 1.85.
The concrete preparation process of present embodiment is:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of deposition are: sputtering power is 73W, and the Ar throughput is 21.0SCCM, and underlayer temperature is 240 ℃, and target-substrate distance is 6.7cm, and sputtering pressure is 0.3Pa, and sedimentation time is 3.3h.
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 47W, and Al target sputtering power is 93W, and the Ar throughput is 17.0SCCM, O
2Throughput is 13.0SCCM, and underlayer temperature is 440 ℃, and target-substrate distance is 7.0cm, and sputtering pressure is 0.3Pa, and sedimentation time is 2.8h.
Step 4, the sapphire that the surface is deposited the CuAlO film carries out annealing in process; The process conditions of annealing are: annealing temperature is 550 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.5h.Obtain the Cu/CuAlO bilayer film.
Embodiment four
The described technical scheme of present embodiment is to be coated with Cu film and CuAlO film on Sapphire Substrate successively.The thickness of Cu film is 360nm, and refractive index is 1.13; The thickness of CuAlO film is 100nm, and refractive index is 2.00.
The concrete preparation process of present embodiment is:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of deposition are: sputtering power is 70W, and the Ar throughput is 24.0SCCM, and underlayer temperature is 300 ℃, and target-substrate distance is 7.0cm, and sputtering pressure is 0.2Pa, and sedimentation time is 4.0h.
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 60W, and Al target sputtering power is 80W, and the Ar throughput is 20.0SCCM, O
2Throughput is 16.0SCCM, and underlayer temperature is 500 ℃, and target-substrate distance is 6.0cm, and sputtering pressure is 0.2Pa, and sedimentation time is 2.5h.
Step 4, the sapphire that the surface is deposited the CuAlO film carries out annealing in process; The process conditions of annealing are: annealing temperature is 600 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.4h.Obtain the Cu/CuAlO bilayer film.
Claims (2)
1. infrared transparent conductive film, it is characterized in that: be coated with Cu film and CuAlO film on Sapphire Substrate successively, wherein the thickness of Cu film is 300～360nm, and refractive index is 1.07～1.13; The thickness of CuAlO film is 100～170nm, and refractive index is 1.70～2.00.
2. a method for preparing the described infrared transparent conductive film of claim 1 is characterized in that, comprises the steps:
Step 1 adopts radio frequency magnetron sputtering method to deposit the Cu film on Sapphire Substrate; The process conditions of deposition are: sputtering power is 70～90W, and the Ar throughput is 17.0～24.0SCCM, and underlayer temperature is 150～300 ℃, and target-substrate distance is 6.2～7.0cm, and sputtering pressure is 0.2～0.5Pa, sedimentation time 2.5～4.0h;
Step 2 is carried out annealing in process to the sapphire that deposits the Cu film; The process conditions of annealing in process are: annealing temperature is 450～600 ℃, and Annealing Protection atmosphere is Ar gas, and annealing time is 0.4～0.6h;
Step 3 adopts radio frequency magnetron sputtering method to deposit the CuAlO film on annealed processing sapphire; The process conditions of deposition are: Cu target sputtering power is 30～60W, and Al target sputtering power is 80～110W, and the Ar throughput is 12.0～20.0SCCM, O
2Throughput is 10.0～16.0SCCM, and underlayer temperature is 350～500 ℃, and target-substrate distance is 6.0～9.0cm, and sputtering pressure is 0.2～0.5Pa, and sedimentation time is 2.5～3.4h;
Step 4 is carried out annealing in process to the sapphire that deposits the CuAlO film; The process conditions of annealing in process are: annealing temperature is 450～600 ℃, and Annealing Protection atmosphere is O
2Gas, annealing time are 0.4～0.6h; Obtain the Cu/CuAlO bilayer film.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280163A (en) * | 2011-05-20 | 2011-12-14 | 西北工业大学 | Infrared transparent conductive film and preparation method thereof |
| CN102586746A (en) * | 2012-02-23 | 2012-07-18 | 吉林大学 | Preparation method of delafossite type copper aluminum oxide infrared transparent conductive film |
| CN105803409A (en) * | 2016-03-23 | 2016-07-27 | 华灿光电股份有限公司 | Method for preparing transparent conducting film |
| CN114032501A (en) * | 2021-11-01 | 2022-02-11 | 吉林大学 | Method for compatibility of far infrared transparency and electric conductivity in thin film material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101609729B (en) * | 2009-07-13 | 2011-08-31 | 浙江大学 | Manufacture method of multilayer transparent electricity conductive film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280163A (en) * | 2011-05-20 | 2011-12-14 | 西北工业大学 | Infrared transparent conductive film and preparation method thereof |
| CN102280163B (en) * | 2011-05-20 | 2013-01-16 | 西北工业大学 | Infrared transparent conductive film and preparation method thereof |
| CN102586746A (en) * | 2012-02-23 | 2012-07-18 | 吉林大学 | Preparation method of delafossite type copper aluminum oxide infrared transparent conductive film |
| CN105803409A (en) * | 2016-03-23 | 2016-07-27 | 华灿光电股份有限公司 | Method for preparing transparent conducting film |
| CN114032501A (en) * | 2021-11-01 | 2022-02-11 | 吉林大学 | Method for compatibility of far infrared transparency and electric conductivity in thin film material |
| CN114032501B (en) * | 2021-11-01 | 2023-09-22 | 吉林大学 | Method for compatible far infrared transparency and conductivity in film material |
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