CN102280163A - Infrared transparent conductive film and preparation method thereof - Google Patents
Infrared transparent conductive film and preparation method thereof Download PDFInfo
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- CN102280163A CN102280163A CN 201110133106 CN201110133106A CN102280163A CN 102280163 A CN102280163 A CN 102280163A CN 201110133106 CN201110133106 CN 201110133106 CN 201110133106 A CN201110133106 A CN 201110133106A CN 102280163 A CN102280163 A CN 102280163A
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Abstract
The invention discloses an infrared transparent conductive film and a preparation method thereof. The preparation method comprises the following steps of: covering an Au grating film layer with thickness of 20-30 nm, period of 500-700 microns and line width of 2.0-4.0 microns on a SiO2 reflection reducing film of a sapphire sample or the sapphire surface, and forming an infrared transparent conductive film by the steps of coating photoresist, pre-baking, exposing, after-baking, depositing the Au film and removing photoresist. The period of the Au grating film is far longer than the wavelength of the infrared light, so the Au grating film has little influence on the infrared optical performance. Meanwhile, the period of the Au grating film is far shorter than the wavelength of the electromagnetic wave, so the Au grating film has good electromagnetic shielding function. Therefore, the Au grating film can be used as the infrared transparent conductive film of the sapphire. In combination with the SiO2-plated infrared reflection-reducing film, the purpose of simultaneously effectively improving the infrared transmissivity and the electromagnetic shielding function of the sapphire substrate can be achieved.
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 3～5 μ m medium wave infrared bands has yittrium oxide, spinelle, nitrogen oxygen aluminium, sapphire etc.Wherein, sapphire has very high hardness, mechanical strength and high temperature stability performance, can bear the thermal shock power that guided missile high-speed flight of new generation produces, and its see through band from ultraviolet, can see infrared, see through the wave band broad, can be fit to multiple aiming means requirements such as optics, electronics.Thereby, sapphire be as medium wave infrared window and head-shield the optimal candidate material (Yin Shengxi, Chu Jianxin. " the novel method of attachment of sapphire dome and metal body is studied ". aviation precision manufacturing technology, 2010,46 (1): 54～57).
The demand for development Infrared Detectors window/hood material of modern military and space technology is except will having good infrared transmittivity, also want to bear the bump of solids such as free dust in high temperature, high pressure, thermal shock, the atmosphere and hail, possess the performance of anti-electromagnetic interference.Be limited to the technology and the level of processing of artificial growing sapphire monocrystal material, sapphire infrared transmittivity can't satisfy actual instructions for use.In addition, the electromagnetic shielding efficiency of sapphire material itself is very low, is easy to be subjected to electromagnetic interference, makes its service behaviour undesirable deviation (service behaviour is by " degradation " in other words) occur.The electronic equipment of detection system inside can produce electromagnetic radiation and might become the clue that the enemy scouts on the other hand, thereby military target is exposed.Thereby how improving sapphire infrared transmittivity and electromagnetic shielding efficiency has effectively become sapphire and has been applied in one of key technology on infrared window/head-shield.
U.S. air-sea tactical operations center adopts radio frequency magnetron sputtering method to prepare individual layer SiO on Sapphire Substrate
2Film and three layers of SiO
2/ Si
3N
4/ SiO
2Laminated film (L.F.Johnson, M.B.Moran. " Compressive Coatings for Strengthened Sapphire " .Proc.of the International Society for Optical Engineering on Window and Dome Technologies and Materials VI, April 1999, Orlando Florida.) is used to improve sapphire infrared transmittivity.This studies show that SiO
2Film and SiO
2/ Si
3N
4/ SiO
2Film system can improve sapphire infrared transmittivity significantly.Applicant and the member of seminar have prepared SiO on Sapphire Substrate
2Film and SiO
2/ Si
3N
4(the L.P.Feng of duplicature system, Z.T.Liu. " Characteristics of Silicon Dioxide Films Prepared on Sapphire " .Material Science and Engineering B, 2005,122 (1): 7～11.L.P.Feng, Z.T.Liu, Q.Li, W.Song. " Investigation of SiO
2/ Si
3N
4Films prepared on sapphire by r.f.magnetron reactive sputtering " .Applied Surface Science, 2006,252 (12): 4064～4070.), discover SiO
2Film and SiO
2/ Si
3N
4Sapphire infrared transmittivity all can improve in duplicature system.But, SiO
2Film, SiO
2/ Si
3N
4/ SiO
2Film system and SiO
2/ Si
3N
4Film system all can not improve sapphire electromagnetic shielding efficiency.
Summary of the invention
In order to overcome the low problem of sapphire electromagnetic shielding efficiency in the prior art, the present invention is being coated with SiO
2A kind of infrared transparent conductive film and preparation method thereof is proposed on the Sapphire Substrate of anti-reflection film.
The technical scheme that the present invention takes is: plate SiO on Sapphire Substrate
2Anti-reflection film forms the sapphire sample; SiO at the sapphire sample
2On the anti-reflection film or sapphire surface cover layer of Au net grid film, form infrared transparent conductive film.The thickness of described Au net grid film is 20～30nm, and the cycle of Au net grid film is 500～700 μ m, and the live width of Au net grid film is 2.0～4.0 μ m.
The present invention also proposes a kind of method for preparing infrared transparent conductive film, may further comprise the steps:
Step 1 is cleaned the sapphire sample.To being coated with SiO
2The sapphire sample of anti-reflection film cleans.The process conditions of cleaning are: the sapphire sample is placed on uses ultrasonic waves for cleaning in the deionized water earlier, hyperacoustic power is 100～200W, and frequency of ultrasonic is 20～24kHz, and scavenging period is 2～4 minutes; Then the sapphire sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, hyperacoustic power is 100～200W, and frequency of ultrasonic is 20～24kHz, and scavenging period is 3～5 minutes, the sapphire sample that obtains cleaning up.
Step 2, resist coating.Adopt the SiO of photoresist spinner at the sapphire sample that cleans up
2Resist coating on the film.The process conditions of resist coating are: at room temperature, the photoresist that drips 3～5ml is at SiO
2On the film, the rotary speed of glue spreader is 3400～3500r/min, and rotational time is 47～53s, obtains scribbling the sapphire sample of photoresist.
Step 3, preceding baking.The sapphire sample that scribbles photoresist is put into baking oven carry out preceding baking.The process conditions of preceding baking are: pre-bake temperature is 105～110 ℃, and preceding baking temperature retention time is 116～120s; Described sapphire sample is taken out air cooling to room temperature, obtain the sapphire sample that scribbles photoresist through preceding baking.
Step 4, exposure.Adopt mask aligner that the sapphire sample that scribbles photoresist through preceding baking is exposed.The process conditions of exposure are: will have the cycle is 500～700 μ m, and live width is the photoresist surface that the mask of 2.0～4.0 μ m is pressed in described sapphire sample, and the time for exposure is 38～42s, obtains the sapphire sample that scribbles photoresist through overexposure.
Step 5 is developed.The sapphire sample that scribbles photoresist through overexposure is developed.The process conditions of developing are: at room temperature, get concentration and be developing solution 20～30ml of 3～4%, described sapphire sample is put into developing solution develop, developing time is 90～96s, obtains the sapphire sample that scribbles photoresist through developing.
Step 6, the back baking.To put into baking oven through the sapphire sample that scribbles photoresist that develops and carry out the back baking.The process conditions of back baking are: the temperature that dry by the fire the back is 108～112 ℃, and the temperature retention time of back baking is 120～126s, then described sapphire sample is taken out air cooling to room temperature, obtains the sapphire sample that scribbles photoresist that dries by the fire through later.
Step 7, deposition Au film.Adopt radio frequency magnetron sputtering method at deposition Au film on the sapphire sample that scribbles photoresist of baking later.The process conditions of rf magnetron sputtering are: sputtering power is 86～90W, the Ar throughput is 13.0～15.0SCCM, underlayer temperature is a room temperature, target-substrate distance is 6.0～6.2cm, sputtering pressure is 0.2～0.3Pa, sedimentation time 5～7min obtains being coated with the sapphire sample that scribbles photoresist of Au net grid film.
Step 8 is removed photoresist.The sapphire sample that scribbles photoresist that is coated with Au net grid film is removed photoresist.Go the process conditions of photoresist to be: the sapphire sample that scribbles photoresist that will be coated with Au net grid film is put into the glue-dispenser ultrasonic waves for cleaning, hyperacoustic power is 200～300W, frequency of ultrasonic is 20～24kHz, scavenging period is 4～6 minutes, obtains removing the sapphire sample that photoresist is coated with Au net grid film.
Step 9 is cleaned.The sapphire sample that is coated with Au net grid film is cleaned.The process conditions of cleaning are: the sapphire sample that will be coated with Au net grid film is placed on uses ultrasonic waves for cleaning in the deionized water, hyperacoustic power is 200～300W, frequency of ultrasonic is 20～24kHz, scavenging period is 6～8 minutes, the sapphire sample that will be coated with Au net grid film then is placed on uses ultrasonic waves for cleaning in the absolute ethyl alcohol, hyperacoustic power is 200～300W, and frequency of ultrasonic is 20～24kHz, scavenging period is 6～8 minutes, obtains infrared transparent conductive film.
The present invention is being coated with SiO
2Deposition Au net grid film on the Sapphire Substrate of anti-reflection film.Because the cycle of Au net grid film is much larger than infrared light wavelength, so Au net grid film is little to the infrared optics performance impact; Simultaneously again since the cycle of Au net grid film much smaller than electromagnetic wavelength, so Au net grid film has good electro-magnetic screen function.Thereby Au net grid film can be used as sapphire infrared transparent conductive film.In conjunction with the SiO that is coated with
2The infrared anti-reflection film can realize improving effectively simultaneously the infrared transmittivity and the electromagnetic shielding efficiency of Sapphire Substrate.
Table 1 for before the embodiment one described same Sapphire Substrate plated film, the two-sided SiO that is coated with
2Behind the anti-reflection film, the two-sided SiO that is coated with
2Anti-reflection film and single face are coated with electromagnetic shielding efficiency and the infrared transmission performance contrast behind the Au net grid film.
The average infrared transmittivities of electromagnetic shielding efficiency (dB) 3～4.5 mu m ranges (%)
Sapphire Substrate 0.13 86.8
SiO
2/ sapphire/SiO
20.10 96.7
Au net grid/SiO
2/ sapphire/SiO
27.12 95.7
The invention will be further described below in conjunction with embodiment.
Embodiment
Embodiment one
Present embodiment is a kind of at the two-sided SiO of being coated with
2The SiO on arbitrary surface of the sapphire sample of anti-reflection film
2Cover layer of Au net grid film on the film again, form infrared transparent conductive film.Desired Au net grid and the SiO of being coated with
2It is 7.12dB that the sapphire of anti-reflection film has electromagnetic shielding efficiency, and the average infrared transmittivity in 3～4.5 mum wavelength scopes is 95.7%.
Upper surface and lower surface in Sapphire Substrate plate SiO respectively
2Anti-reflection film forms the sapphire sample.In the present embodiment, be upper surface covering layer of Au net grid film at the sapphire sample.Be plated in the SiO on the Sapphire Substrate
2The thickness of film is 650nm, and refractive index is 1.41; The thickness of Au net grid film is 20nm, and the cycle of Au net grid film is 700 μ m, and the live width of Au net grid film is 2.0 μ m.
The concrete preparation process of present embodiment is:
Step 1 is cleaned the sapphire sample.To the two-sided SiO that is coated with
2The sapphire sample of anti-reflection film, i.e. SiO
2/ sapphire/SiO
2Sample cleans.The process conditions of cleaning are: earlier with SiO
2/ sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 200W, and frequency of ultrasonic is 24kHz, and scavenging period is 2 minutes, then with SiO
2/ sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 200W, and frequency of ultrasonic is 24kHz, and scavenging period is 3 minutes, the SiO that obtains cleaning up
2/ sapphire/SiO
2Sample.
Step 2, resist coating.The SiO that adopts photoresist spinner cleaning up
2/ sapphire/SiO
2The upper surface SiO of sample
2Resist coating on the film; The process conditions of resist coating are: at room temperature, the JHF-30 photoresist that drips 3ml is at SiO
2On the film, the rotary speed of glue spreader is 3400r/min, and rotational time is 47s, obtains scribbling the SiO of photoresist
2/ sapphire/SiO
2Sample, i.e. photoresist/SiO
2/ sapphire/SiO
2Sample.
Step 3, preceding baking.With photoresist/SiO
2/ sapphire/SiO
2Sample is put into baking oven and is carried out preceding baking; The process conditions of preceding baking are: pre-bake temperature is 105 ℃, and preceding baking temperature retention time is 120s, then with photoresist/SiO
2/ sapphire/SiO
2Sample takes out air cooling to room temperature, obtains the photoresist/SiO through preceding baking
2/ sapphire/SiO
2Sample.
Step 4, exposure.Adopt mask aligner to photoresist/SiO through preceding baking
2/ sapphire/SiO
2Sample exposes; The process conditions of exposure are: will have the cycle is 700 μ m, and live width is that the mask of 2.0 μ m is pressed in photoresist/SiO
2/ sapphire/SiO
2The photoresist surface of sample, the time for exposure is 38s, obtains the photoresist/SiO through overexposure
2/ sapphire/SiO
2Sample.
Step 5 is developed.To photoresist/SiO through overexposure
2/ sapphire/SiO
2Sample develops; The process conditions of developing are: at room temperature, get concentration and be 3% FX-C type developing solution 20ml, and will be through the photoresist/SiO of overexposure
2/ sapphire/SiO
2Sample is put into developing solution and is developed, and developing time is 90s, obtains the photoresist/SiO through developing
2/ sapphire/SiO
2Sample.
Step 6, the back baking.Will be through the photoresist/SiO that develops
2/ sapphire/SiO
2Sample is put into baking oven and is carried out the back baking; The process conditions of back baking are: the temperature of back baking is 108 ℃, and the temperature retention time of back baking is 126s, then with photoresist/SiO
2/ sapphire/SiO
2Sample takes out air cooling to room temperature, obtains the photoresist/SiO that dries by the fire through later
2/ sapphire/SiO
2Sample.
Step 7, deposition Au film.Adopt radio frequency magnetron sputtering method at photoresist/SiO through drying by the fire later
2/ sapphire/SiO
2Deposition Au film on the sample; The process conditions of rf magnetron sputtering are: sputtering power is 86W, and the Ar throughput is 13.0SCCM, and underlayer temperature is a room temperature, and target-substrate distance is 6.2cm, and sputtering pressure is 0.3Pa, and sedimentation time 5min obtains being coated with the photoresist/SiO of Au net grid film
2/ sapphire/SiO
2Sample.
Step 8 is removed photoresist.To being coated with the photoresist/SiO of Au net grid film
2/ sapphire/SiO
2Sample removes photoresist; Go the process conditions of photoresist to be: the photoresist/SiO that will be coated with Au net grid film
2/ sapphire/SiO
2Sample is put into SN-01 type glue-dispenser ultrasonic waves for cleaning, and hyperacoustic power is 300W, and frequency of ultrasonic is 24kHz, and scavenging period is 4 minutes, obtains removing the SiO that photoresist is coated with Au net grid film
2/ sapphire/SiO
2Sample, i.e. Au net grid/SiO
2/ sapphire/SiO
2Sample.
Step 9 is cleaned.To Au net grid/SiO
2/ sapphire/SiO
2Sample cleans; The process conditions of cleaning are: with Au net grid/SiO
2/ sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 300W, and frequency of ultrasonic is 24kHz, and scavenging period is 6 minutes, then with Au net grid/SiO
2/ sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 300W, and frequency of ultrasonic is 24kHz, and scavenging period is 6 minutes, obtains infrared transparent conductive film.
Embodiment two
Present embodiment is a kind ofly to be coated with SiO at single face
2The SiO of the sapphire sample of anti-reflection film
2Cover layer of Au net grid film on the film again, form infrared transparent conductive film.Desired Au net grid and the SiO of being coated with
2It is 7.21dB that the sapphire of anti-reflection film has electromagnetic shielding efficiency, and the average infrared transmittivity in 3～4.5 mum wavelength scopes is 90.4%.
Upper surface in Sapphire Substrate plates SiO
2Anti-reflection film forms the sapphire sample.In the present embodiment, be upper surface SiO at the sapphire sample
2Cover layer of Au net grid film on the anti-reflection film again.Be plated in the SiO on the Sapphire Substrate
2The thickness of film is 640nm, and refractive index is 1.38; The thickness of Au net grid film is 25nm, and the cycle of Au net grid film is 600 μ m, and the live width of Au net grid film is 3.0 μ m.
The concrete preparation process of present embodiment is:
Step 1 is cleaned the sapphire sample.Upper surface is coated with SiO
2The sapphire sample of anti-reflection film, i.e. SiO
2/ sapphire sample cleans.The process conditions of cleaning are: earlier with SiO
2/ sapphire sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 150W, and frequency of ultrasonic is 22kHz, and scavenging period is 3 minutes, then with SiO
2/ sapphire sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 150W, and frequency of ultrasonic is 22kHz, and scavenging period is 4 minutes, the SiO that obtains cleaning up
2/ sapphire sample.
Step 2, resist coating.The SiO that adopts photoresist spinner cleaning up
2The upper surface SiO of/sapphire sample
2Resist coating on the film; The process conditions of resist coating are: at room temperature, the NR9-1000PY photoresist that drips 4ml is at SiO
2On the film, the rotary speed of glue spreader is 3450r/min, and rotational time is 50s, obtains scribbling the SiO of photoresist
2/ sapphire sample, i.e. photoresist/SiO
2/ sapphire sample.
Step 3, preceding baking.With photoresist/SiO
2/ sapphire sample is put into baking oven and is carried out preceding baking; The process conditions of preceding baking are: pre-bake temperature is 107 ℃, and preceding baking temperature retention time is 118s, then with photoresist/SiO
2/ sapphire sample takes out air cooling to room temperature, obtains the photoresist/SiO through preceding baking
2/ sapphire sample.
Step 4, exposure.Adopt mask aligner to photoresist/SiO through preceding baking
2/ sapphire sample exposes; The process conditions of exposure are: will have the cycle is 600 μ m, and live width is that the mask of 3.0 μ m is pressed in photoresist/SiO
2The photoresist surface of/sapphire sample, the time for exposure is 40s, obtains the photoresist/SiO through overexposure
2/ sapphire sample.
Step 5 is developed.To photoresist/SiO through overexposure
2/ sapphire sample develops; The process conditions of developing are: at room temperature, get concentration and be 3.5% RD6 type developing solution 25ml, and will be through the photoresist/SiO of overexposure
2/ sapphire sample is put into developing solution and is developed, and developing time is 93s, obtains the photoresist/SiO through developing
2/ sapphire sample.
Step 6, the back baking.Will be through the photoresist/SiO that develops
2/ sapphire sample is put into baking oven and is carried out the back baking; The process conditions of back baking are: the temperature of back baking is 110 ℃, and the temperature retention time of back baking is 124s, then with photoresist/SiO
2/ sapphire sample takes out air cooling to room temperature, obtains the photoresist/SiO that dries by the fire through later
2/ sapphire sample.
Step 7, deposition Au film.Adopt radio frequency magnetron sputtering method at photoresist/SiO through drying by the fire later
2Deposition Au film on the/sapphire sample; The process conditions of rf magnetron sputtering are: sputtering power is 88W, and the Ar throughput is 14.0SCCM, and underlayer temperature is a room temperature, and target-substrate distance is 6.1cm, and sputtering pressure is 0.25Pa, and sedimentation time 6min obtains being coated with the photoresist/SiO of Au net grid film
2/ sapphire sample.
Step 8 is removed photoresist.To being coated with the photoresist/SiO of Au net grid film
2/ sapphire sample removes photoresist; Go the process conditions of photoresist to be: the photoresist/SiO that will be coated with Au net grid film
2/ sapphire sample is put into RR4 type glue-dispenser ultrasonic waves for cleaning, and hyperacoustic power is 250W, and frequency of ultrasonic is 22kHz, and scavenging period is 5 minutes, obtains removing the SiO that photoresist is coated with Au net grid film
2/ sapphire sample, i.e. Au net grid/SiO
2/ sapphire sample.
Step 9 is cleaned.To Au net grid/SiO
2/ sapphire sample cleans; The process conditions of cleaning are: with Au net grid/SiO
2/ sapphire sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 250W, and frequency of ultrasonic is 22kHz, and scavenging period is 7 minutes, then with Au net grid/SiO
2/ sapphire sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 250W, and frequency of ultrasonic is 22kHz, and scavenging period is 7 minutes, obtains infrared transparent conductive film.
Embodiment three
Present embodiment is a kind of layer of Au net grid film that covers on the sapphire specimen surface, forms infrared transparent conductive film.A surface of described sapphire sample is coated with SiO
2Anti-reflection film; Au net grid film directly overlays sapphire surface.Desired Au net grid and the SiO of being coated with
2It is 7.45dB that the sapphire of anti-reflection film has electromagnetic shielding efficiency, and the average infrared transmittivity in 3～4.5 mum wavelength scopes is 90.1%.
Be plated in the SiO on the Sapphire Substrate
2The thickness of film is 660nm, and refractive index is 1.40; The thickness of Au net grid film is 30nm, and the cycle of Au net grid film is 500 μ m, and the live width of Au net grid film is 4.0 μ m.
The concrete preparation process of present embodiment is:
Step 1 is cleaned the sapphire sample.Lower surface is coated with SiO
2The sapphire sample of anti-reflection film, i.e. sapphire/SiO
2Sample cleans.The process conditions of cleaning are: earlier with sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 100W, and frequency of ultrasonic is 20kHz, and scavenging period is 4 minutes, then with sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 100W, and frequency of ultrasonic is 20kHz, and scavenging period is 5 minutes, the sapphire/SiO that obtains cleaning up
2Sample.
Step 2, resist coating.Sapphire/the SiO that adopts photoresist spinner cleaning up
2Resist coating on the upper surface sapphire of sample; The process conditions of resist coating are: at room temperature, the RFJ-220 photoresist that drips 5ml is at SiO
2On the film, the rotary speed of glue spreader is 3500r/min, and rotational time is 53s, obtains scribbling the sapphire/SiO of photoresist
2Sample, i.e. photoresist/sapphire/SiO
2Sample.
Step 3, preceding baking.With photoresist/sapphire/SiO
2Sample is put into baking oven and is carried out preceding baking; The process conditions of preceding baking are: pre-bake temperature is 110 ℃, and preceding baking temperature retention time is 116s, then with photoresist/sapphire/SiO
2Sample takes out air cooling to room temperature, obtains the photoresist/sapphire/SiO through preceding baking
2Sample.
Step 4, exposure.Adopt mask aligner to photoresist/sapphire/SiO through preceding baking
2Sample exposes; The process conditions of exposure are: will have the cycle is 500 μ m, and live width is that the mask of 4.0 μ m is pressed in photoresist/sapphire/SiO
2The photoresist surface of sample, the time for exposure is 42s, obtains the photoresist/sapphire/SiO through overexposure
2Sample.
Step 5 is developed.To photoresist/sapphire/SiO through overexposure
2Sample develops; The process conditions of developing are: at room temperature, get concentration and be 4% RFX type developing solution 30ml, and will be through the photoresist/sapphire/SiO of overexposure
2Sample is put into developing solution and is developed, and developing time is 96s, obtains the photoresist/sapphire/SiO through developing
2Sample.
Step 6, the back baking.Will be through the photoresist/sapphire/SiO that develops
2Sample is put into baking oven and is carried out the back baking; The process conditions of back baking are: the temperature of back baking is 112 ℃, and the temperature retention time of back baking is 120s, then with photoresist/sapphire/SiO
2Sample takes out air cooling to room temperature, obtains the photoresist/sapphire/SiO that dries by the fire through later
2Sample.
Step 7, deposition Au film.Adopt radio frequency magnetron sputtering method at photoresist/sapphire/SiO through drying by the fire later
2Deposition Au film on the sample; The process conditions of rf magnetron sputtering are: sputtering power is 90W, and the Ar throughput is 15.0SCCM, and underlayer temperature is a room temperature, and target-substrate distance is 6.0cm, and sputtering pressure is 0.2Pa, and sedimentation time 7min obtains being coated with the photoresist/sapphire/SiO of Au net grid film
2Sample.
Step 8 is removed photoresist.To being coated with the photoresist/sapphire/SiO of Au net grid film
2Sample removes photoresist; Go the process conditions of photoresist to be: the photoresist/sapphire/SiO that will be coated with Au net grid film
2Sample is put into SN-01 type glue-dispenser ultrasonic waves for cleaning, and hyperacoustic power is 200W, and frequency of ultrasonic is 20kHz, and scavenging period is 6 minutes, obtains removing sapphire/SiO that photoresist is coated with Au net grid film
2Sample, i.e. Au net grid/sapphire/SiO
2Sample.
Step 9 is cleaned.To Au net grid/sapphire/SiO
2Sample cleans; The process conditions of cleaning are: with Au net grid/sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the deionized water, and hyperacoustic power is 200W, and frequency of ultrasonic is 20kHz, and scavenging period is 8 minutes, then with Au net grid/sapphire/SiO
2Sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, and hyperacoustic power is 200W, and frequency of ultrasonic is 20kHz, and scavenging period is 8 minutes, obtains infrared transparent conductive film.
Claims (2)
1. infrared transparent conductive film, the single or double of Sapphire Substrate plates SiO
2Anti-reflection film forms the sapphire sample; It is characterized in that: at the SiO of sapphire sample
2On the anti-reflection film or sapphire surface cover layer of Au net grid film, formed infrared transparent conductive film; The thickness of Au net grid film is 20～30nm, and the cycle of Au net grid film is 500～700 μ m, and the live width of Au net grid film is 2.0～4.0 μ m.
2. a method for preparing the described infrared transparent conductive film of claim 1 is characterized in that, comprises the steps: step 1, cleans the sapphire sample; To being coated with SiO
2The sapphire sample of anti-reflection film cleans; The process conditions of cleaning are: the sapphire sample is placed on uses ultrasonic waves for cleaning in the deionized water earlier, hyperacoustic power is 100～200W, and frequency of ultrasonic is 20～24kHz, and scavenging period is 2～4 minutes; Then the sapphire sample is placed on and uses ultrasonic waves for cleaning in the absolute ethyl alcohol, hyperacoustic power is 100～200W, and frequency of ultrasonic is 20～24kHz, and scavenging period is 3～5 minutes, the sapphire sample that obtains cleaning up;
Step 2, resist coating; Adopt the SiO of photoresist spinner at the sapphire sample that cleans up
2Resist coating on the film; The process conditions of resist coating are: at room temperature, the photoresist that drips 3～5ml is at SiO
2On the film, the rotary speed of glue spreader is 3400～3500r/min, and rotational time is 47～53s, obtains scribbling the sapphire sample of photoresist;
Step 3, preceding baking; The sapphire sample that scribbles photoresist is put into baking oven carry out preceding baking; The process conditions of preceding baking are: pre-bake temperature is 105～110 ℃, and preceding baking temperature retention time is 116～120s; Described sapphire sample is taken out air cooling to room temperature, obtain the sapphire sample that scribbles photoresist through preceding baking;
Step 4, exposure; Adopt mask aligner that the sapphire sample that scribbles photoresist through preceding baking is exposed; The process conditions of exposure are: will have the cycle is 500～700 μ m, and live width is the photoresist surface that the mask of 2.0～4.0 μ m is pressed in described sapphire sample, and the time for exposure is 38～42s, obtains the sapphire sample that scribbles photoresist through overexposure;
Step 5 is developed; The sapphire sample that scribbles photoresist through overexposure is developed; The process conditions of developing are: at room temperature, get concentration and be developing solution 20～30ml of 3～4%, described sapphire sample is put into developing solution develop, developing time is 90～96s, obtains the sapphire sample that scribbles photoresist through developing;
Step 6, the back baking; To put into baking oven through the sapphire sample that scribbles photoresist that develops and carry out the back baking; The process conditions of back baking are: the temperature that dry by the fire the back is 108～112 ℃, and the temperature retention time of back baking is 120～126s, then described sapphire sample is taken out air cooling to room temperature, obtains the sapphire sample that scribbles photoresist that dries by the fire through later;
Step 7, deposition Au film; Adopt radio frequency magnetron sputtering method at deposition Au film on the sapphire sample that scribbles photoresist of baking later; The process conditions of rf magnetron sputtering are: sputtering power is 86～90W, the Ar throughput is 13.0～15.0SCCM, underlayer temperature is a room temperature, target-substrate distance is 6.0～6.2cm, sputtering pressure is 0.2～0.3Pa, sedimentation time 5～7min obtains being coated with the sapphire sample that scribbles photoresist of Au net grid film;
Step 8 is removed photoresist; The sapphire sample that scribbles photoresist that is coated with Au net grid film is removed photoresist; Go the process conditions of photoresist to be: the sapphire sample that scribbles photoresist that will be coated with Au net grid film is put into the glue-dispenser ultrasonic waves for cleaning, hyperacoustic power is 200～300W, frequency of ultrasonic is 20～24kHz, scavenging period is 4～6 minutes, obtains removing the sapphire sample that photoresist is coated with Au net grid film;
Step 9 is cleaned; The sapphire sample that is coated with Au net grid film is cleaned; The process conditions of cleaning are: the sapphire sample that will be coated with Au net grid film is placed on uses ultrasonic waves for cleaning in the deionized water, hyperacoustic power is 200～300W, frequency of ultrasonic is 20～24kHz, scavenging period is 6～8 minutes, the sapphire sample that will be coated with Au net grid film then is placed on uses ultrasonic waves for cleaning in the absolute ethyl alcohol, hyperacoustic power is 200～300W, and frequency of ultrasonic is 20～24kHz, scavenging period is 6～8 minutes, obtains infrared transparent conductive film.
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| CN105887032A (en) * | 2016-05-10 | 2016-08-24 | 中国建筑材料科学研究总院 | Shielding optical window and preparation method thereof |
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| CN110838390A (en) * | 2019-11-21 | 2020-02-25 | 武汉大学 | Method for preparing patterned transparent conductive film by laser |
| CN110838390B (en) * | 2019-11-21 | 2021-08-24 | 武汉大学 | Method for preparing patterned transparent conductive film by laser |
| CN111025446A (en) * | 2019-12-10 | 2020-04-17 | 西安应用光学研究所 | Infrared binary optical device and electromagnetic shielding mesh grid preparation method |
| CN111025446B (en) * | 2019-12-10 | 2022-03-15 | 西安应用光学研究所 | Infrared binary optical device and electromagnetic shielding mesh grid preparation method |
| CN111276277A (en) * | 2020-02-12 | 2020-06-12 | 哈尔滨工业大学 | Window with infrared transparent conductive function |
| CN111276277B (en) * | 2020-02-12 | 2021-06-29 | 哈尔滨工业大学 | Window with infrared transparent conductive function |
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