CN102605333A - Preparation method for tantalum oxide film with high laser damage threshold under high-temperature environment - Google Patents
Preparation method for tantalum oxide film with high laser damage threshold under high-temperature environment Download PDFInfo
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Abstract
The invention relates to a preparation method for a tantalum oxide film with a high laser damage threshold under a high-temperature environment and belongs to the preparation method for an optical film. The preparation method comprises the following steps: plating a tantalum oxide film on a clean substrate according to a double ion beam sputtering method; performing post-processing on a prepared film in laser pre-processing and annealing manner, thereby achieving better functions of repairing film defect and relieving film stress; and preparing a laser film capable of being applied to high-temperature environment. The preparation method provided by the invention has the advantages that: 1) the film prepared according to the double ion beam sputtering method is compact, the characteristic of easiness in moisture absorption of a loosened film prepared according to an electronic beam preparation method is improved, and the stability is better; 2) the laser pre-processing and annealing combined method is adopted, thereby overcoming the limitation caused by traditionally adopting a single method, and being beneficial to greatly increasing the threshold; and 3) the film prepared according to the method can be used under a high-temperature environment with the highest temperature at 350 DEG C, and the problem of the prior art that only the laser film used under room temperature can be prepared is solved.
Description
Technical field
The invention belongs to the preparation method of optical thin film, be specifically related to have under a kind of hot environment the preparation method of high laser damage threshold tantalum oxide film.
Background technology
The foundation of high-power laser system and the proposition of laser ignited have proposed more and more harsher requirement to the optical thin film performance, particularly require it to have superpower resisting laser damage ability.The Research on injury threshold emphasis mainly concentrates on film characteristics and laser parameter for many years, has studied base reservoir temperature, oxygen partial pressure and sedimentation rate in the electron beam evaporation process to Ta like people such as Milam
2O
5/ SiO
2The influence of anti-reflection film damage threshold (Applied Optics, 1982,21,3689～3694.), people such as Abromavicius have studied sedimentation rate in the ion beam assisted depositing method, base reservoir temperature and ion beam current energy to Ta
2O
5/ SiO
2The influence of high-reflecting film threshold value (Proc.SPIE, 2007,6403; 640315); People such as horse equality people and Riede have studied the damage from laser of dissimilar films in the vacuum (light laser and particle beam, 2009,21; 1829～1832), people such as Shen Jun has adopted Prepared by Sol Gel Method and has had a ZIRCONIUM DIOXIDE 99.5 film (CN15553220A) of high laser damage threshold.But the laser deflection Value Data in these researchs is all measured at normal temperatures.
Along with the expansion in laser applications field, temperature factor is more and more outstanding to the influence of membrane laser damage.Under the background that develops rapidly in current space technology, the space laser device just needs the influence of account temperature, because space middle-jiao yang, function of the spleen and stomach light direct beam surface temperature can rise to 250 ℃; And laser lithography technology expectation of future generation is broken through 20 nano-photoetching nodes, and thin-film component wherein need bear the high temperature of hundreds of degree for a long time.In these cases, the conventional laser film that under normal temperature condition, uses just is difficult to be suitable for.The correlative study that is applied to have under the hot environment high laser damage threshold film does not up to now see that report is arranged.
Summary of the invention
The objective of the invention is to provide the preparation method who has high laser damage threshold tantalum oxide film under a kind of hot environment, solves the pyritous problem that the laser film element can not bear hundreds of degree for a long time.
The objective of the invention is to provide a kind of preparation method of tantalum oxide film of high laser damage threshold, its concrete steps are:
One, substrate is soaked in the scavenging solution, ultrasonic cleaning 5～30min rinses well with deionized water then, dries up with high pure nitrogen at last;
Two, the High-purity Tantalum target of employing 99.999% is with double ion beam sputtered method plated film in the substrate of above-mentioned processing; The base vacuum degree is 5 * 10
-4～1 * 10
-5Pa, storing temperature are 60～150 ℃, and it is 1 * 10 that oxygenation is pressed
-2～1 * 10
-1Pa, the argon flow amount of sputtering source are 5～90mL/min, and the argon flow amount of radio frequency neutralizer is 0.5～30mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.1～1, earlier the tantalum target are carried out 5min before the sputter and clean, and begin to be coated with film then;
Three, the film that is coated with is carried out laser pre-treated, the focal beam spot diameter is 50～900 μ m, and pretreated energy size is confirmed according to the laser damage threshold of film under the normal temperature.Wherein the laser damage threshold method of testing of film is following under the normal temperature: choosing energy density is the laser irradiation testing sample of 1～50J/cm2; Measure 10 points with the mode of 1-on-1; Draw the probability of damage; Change its energy density then; Obtain the damage probability under the different-energy density laser; Choose 10 energy probability, promptly measure 10 * 10 points altogether; By computer the laser energy density that at every turn acts on the sample is gathered in real time; According to the damage probability in each energy density section, the laser energy density when drawing the zero probability damage by the linear fit method of mapping is the instant damage threshold of laser irradiation sample under the normal temperature then; Adopt the step pretreatment mode; Detailed process is: the preliminary treatment energy to every of film surface begins from 30% of normal temperature laser damage threshold; Increase by 10% then at every turn; Step is energization gradually; Stop up to increasing to 80%; Begin the preliminary treatment of next point then, film surface is all handled always;
Four, pretreated tantalum-oxide film is carried out anneal in atmosphere, annealing temperature is 200～400 ℃, and temperature rise rate is 0.01～20 ℃/min, and soaking time is 1～50h.
Described substrate is BK7 glass or quartz.
Described scavenging solution is any in sherwood oil, the acetone or alcohol, or wherein any two kinds of described sherwood oil, acetone and ethanol, with the mixture of arbitrary volume ratio.
Described annealing atmosphere be oxygen, nitrogen, argon gas or airborne any.
Beneficial effect owing to adopted such scheme, uses the tantalum oxide with high crystal phase transition temperature as Coating Materials, utilizes the high-temperature resistance of tantalum oxide material, helps improving the damage threshold of the film of preparation.Laser pre-treated and the post-treating method of annealing and combining have been adopted simultaneously; Can better repair the gentle degrading film stress of film defects; Thereby improved the laser damage threshold under the hot environment; Solve the pyritous problem that the laser film element can not bear hundreds of degree for a long time, reached the object of the invention.
The present invention has following advantage:
1, the present invention adopts double ion beam sputtered method, and the film of preparation is dense, and the loose film that has improved the preparation of methods such as electron beam preparation is prone to the characteristics of the moisture absorption, has better stability.
2, the method that has adopted laser pre-treated and annealing to combine among the present invention has been improved a limitation with a kind of method in the past, helps promoting to a greater extent threshold value.
3, the film of this method preparation can use under the highest 350 ℃ hot environment, has solved the technological in the past problem that can only prepare the laser film that uses under the normal temperature.
Embodiment
Through embodiment the present invention is detailed below.
Embodiment 1: the BK7 substrate of glass is soaked in the sherwood oil, and ultrasonic cleaning 15min rinses well with deionized water then, dries up with high pure nitrogen at last.Adopt double ion beam sputtered method in the BK7 substrate of cleaning, to be coated with tantalum-oxide film, the base vacuum degree is 2 * 10
-4Pa, storing temperature are 80 ℃, and it is 5 * 10 that oxygenation is pressed
-2Pa, the argon flow amount of sputtering source are 15mL/min, and the argon flow amount of radio frequency neutralizer is 5mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.5, earlier the tantalum target are carried out 5min before the sputter and clean, and are coated with film then.The tantalum oxide film for preparing is carried out the standard damage threshold test under the normal temperature; Mode with 1-on-1; According to the ISO11254-1 standard, the energy density during with zero damage probability is as the laser damage threshold of film, and the threshold value under the 1064nm laser that records is 18J/cm
2With the above-mentioned threshold value that records is standard, and the tantalum oxide film is carried out laser pre-treated, and optical maser wavelength 1064nm, focal beam spot diameter are 200 μ m, adopts the step type pretreatment mode, to the pre-treatment energy of every of film surface from 5.4J/cm
21.8J/cm is pressed in beginning then
2The step energization, up to increasing to 14.4J/cm
2Stop, beginning the pre-treatment of next point then, film surface is all handled always.Tantalum-oxide film after the laser pre-treated is carried out anneal in air, annealing temperature is 350 ℃, and temperature rise rate is 5 ℃/min, and soaking time is 10h.
The laser damage threshold test of film under hot environment carried out on self-built high-temperature laser damage threshold test platform: 350 ℃ of design temperatures; The employing wavelength is that the electric-optically Q-switched single-mode laser of Nd:YAG of 1064nm is measured the laser damage threshold of film; The light beam vertical incidence; Repetition rate 1Hz, PW 12 ns, the sample surfaces spot size is 0.467mm.Laser is spaced apart 1.5mm at the irradiation of sample surfaces, adopts the mode of 1-on-1 to test, and measures 10 * 10 points altogether.With online microscope judgment means degree of impairment is monitored in real time in the experiment; Laser energy to act on the sample is at every turn gathered through computingmachine in real time; Then according at the damage probability of each energy section, the laser damage threshold of film when drawing the zero probability damage through the linear fit method of mapping.
Test result shows that under 350 ℃ temperature, the damage threshold of film under 1064nm laser is 11J/cm
2
Embodiment 2: quartz substrate is soaked in the mixed solution of sherwood oil and acetone, both volume ratios are 1:1, and ultrasonic cleaning 20min rinses well with deionized water then, dries up with high pure nitrogen at last.Adopt double ion beam sputtered method on the quartz substrate of cleaning, to be coated with tantalum-oxide film, the base vacuum degree is 2.4 * 10
-4Pa, storing temperature are 120 ℃, and it is 8 * 10 that oxygenation is pressed
-2Pa, the argon flow amount of sputtering source are 20mL/min, and the argon flow amount of radio frequency neutralizer is 4mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.4, earlier the tantalum target are carried out 5min before the sputter and clean, and are coated with film then.The tantalum oxide film for preparing is carried out the standard damage threshold test under the normal temperature; Mode with 1-on-1; According to the ISO11254-1 standard, the energy density during with zero damage probability is as the laser damage threshold of film, and the threshold value under the 1064nm laser that records is 20J/cm
2With the above-mentioned threshold value that records is standard, and the tantalum oxide film is carried out laser pre-treated, and optical maser wavelength 1064nm, focal beam spot diameter are 180 μ m, adopts the step type pretreatment mode, to the pre-treatment energy of every of film surface from 6J/cm
22J/cm is pressed in beginning then
2The step energization, up to increasing to 16J/cm
2Stop, beginning the pre-treatment of next point then, film surface is all handled always.Tantalum-oxide film after the laser pre-treated is carried out anneal in air, annealing temperature is 400 ℃, and temperature rise rate is 2 ℃/min, and soaking time is 12h.Test result shows that under 300 ℃ temperature, the damage threshold of film under 1064nm laser is 15J/cm
2
Embodiment 3: quartz substrate is soaked in acetone and the alcoholic acid mixed solution, and both volume ratios are 8:1, and ultrasonic cleaning 30min rinses well with deionized water then, dries up with high pure nitrogen at last.Adopt double ion beam sputtered method on the quartz substrate of cleaning, to be coated with tantalum-oxide film, the base vacuum degree is 1 * 10
-5Pa, storing temperature are 150 ℃, and it is 6 * 10 that oxygenation is pressed
-2Pa, the argon flow amount of sputtering source are 80mL/min, and the argon flow amount of radio frequency neutralizer is 25mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.1, earlier the tantalum target are carried out 5min before the sputter and clean, and are coated with film then.The tantalum oxide film for preparing is carried out the standard damage threshold test under the normal temperature; Mode with 1-on-1; According to the ISO11254-1 standard, the energy density during with zero damage probability is as the laser damage threshold of film, and the threshold value under the 532nm laser that records is 10J/cm
2With the above-mentioned threshold value that records is standard, and the tantalum oxide film is carried out laser pre-treated, and optical maser wavelength 532nm, focal beam spot diameter are 800 μ m, adopts the step type pretreatment mode, to the pre-treatment energy of every of film surface from 3J/cm
21J/cm is pressed in beginning then
2The step energization, up to increasing to 8J/cm
2Stop, beginning the pre-treatment of next point then, film surface is all handled always.Tantalum-oxide film after the laser pre-treated is carried out anneal in air, annealing temperature is 250 ℃, and temperature rise rate is 20 ℃/min, and soaking time is 12h.Test result shows that under 250 ℃ temperature, the damage threshold of film under 532nm laser is 8J/cm
2
Embodiment 4: the BK7 substrate of glass is soaked in the ethanol, and ultrasonic cleaning 5min rinses well with deionized water then, dries up with high pure nitrogen at last.Adopt double ion beam sputtered method in the BK7 substrate of cleaning, to be coated with tantalum-oxide film, the base vacuum degree is 5 * 10
-4Pa, storing temperature are 60 ℃, and it is 5 * 10 that oxygenation is pressed
-2Pa, the argon flow amount of sputtering source are 10mL/min, and the argon flow amount of radio frequency neutralizer is 15mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.6, earlier the tantalum target are carried out 5min before the sputter and clean, and are coated with the tantalum oxide film then.On the tantalum oxide film that is coated with, be coated with the layer of silicon dioxide film, alternately be coated with for 10 cycles then, the film of preparation is 99% at the reflectivity of 1064nm.The film for preparing is carried out the standard damage threshold test under the normal temperature, and with the mode of 1-on-1, according to the ISO11254-1 standard, the energy density during with zero damage probability is as the laser damage threshold of film, and the threshold value under the 1064nm laser that records is 35J/cm
2With the above-mentioned threshold value that records is standard, and the tantalum oxide film is carried out laser pre-treated, and optical maser wavelength 1064nm, focal beam spot diameter are 300 μ m, adopts the step type pretreatment mode, to the pre-treatment energy of every of film surface from 10.5J/cm
23.5J/cm is pressed in beginning then
2The step energization, up to increasing to 28J/cm
2Stop, beginning the pre-treatment of next point then, film surface is all handled always.Tantalum-oxide film after the laser pre-treated is carried out anneal in air, annealing temperature is 200 ℃, and temperature rise rate is 0.01 ℃/min, and soaking time is 6h.Test result shows that under 200 ℃ temperature, the damage threshold of film under 1064nm laser is 24J/cm
2
Embodiment 5: quartz substrate is soaked in the acetone, and ultrasonic cleaning 10min rinses well with deionized water then, dries up with high pure nitrogen at last.Adopt double ion beam sputtered method on the quartz substrate of cleaning, to be coated with tantalum-oxide film, the base vacuum degree is 6 * 10
-4Pa, storing temperature are 110 ℃, and it is 3.2 * 10 that oxygenation is pressed
-2Pa, the argon flow amount of sputtering source are 16mL/min, and the argon flow amount of radio frequency neutralizer is 3mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.4, earlier the tantalum target are carried out 5min before the sputter and clean, and are coated with the tantalum oxide film then.On the tantalum oxide film that is coated with, be coated with certain thickness silicon-dioxide and make that the film of preparation is 98% in the transmitance of 1064nm.The film for preparing is carried out the standard damage threshold test under the normal temperature, and with the mode of 1-on-1, according to the ISO11254-1 standard, the energy density during with zero damage probability is as the laser damage threshold of film, and the threshold value under the 1064nm laser that records is 22J/cm
2With the above-mentioned threshold value that records is standard, and the tantalum oxide film is carried out laser pre-treated, and optical maser wavelength 1064nm, focal beam spot diameter are 350 μ m, adopts the step type pretreatment mode, to the pre-treatment energy of every of film surface from 6.6J/cm
22.2J/cm is pressed in beginning then
2The step energization, up to increasing to 17.6J/cm
2Stop, beginning the pre-treatment of next point then, film surface is all handled always.Tantalum-oxide film after the laser pre-treated is carried out anneal in air, annealing temperature is 220 ℃, and temperature rise rate is 0.01 ℃/min, and soaking time is 10h.Test result shows that under 220 ℃ temperature, the damage threshold of film under 1064nm laser is 17J/cm
2
Claims (4)
1. have the preparation method of high laser damage threshold tantalum oxide film under the hot environment, it is characterized in that: its concrete steps are:
One, substrate is soaked in the scavenging solution, ultrasonic cleaning 5～30min rinses well with deionized water then, dries up with high pure nitrogen at last;
Two, the High-purity Tantalum target of employing 99.999% is with double ion beam sputtered method plated film in the substrate of above-mentioned processing; The base vacuum degree is 5 * 10
-4～1 * 10
-5Pa, storing temperature are 60～150 ℃, and it is 1 * 10 that oxygenation is pressed
-2～1 * 10
-1Pa, the argon flow amount of sputtering source are 5～90mL/min, and the argon flow amount of radio frequency neutralizer is 0.5～30mL/min, and the argon gas of second source and the throughput ratio of oxygen are 0.1～1, earlier the tantalum target are carried out 5min before the sputter and clean, and begin to be coated with film then;
Three, the film that is coated with is carried out laser pre-treated, the focal beam spot diameter is 50～900 μ m, and pretreated energy size is confirmed according to the laser damage threshold of film under the normal temperature;
Wherein the laser damage threshold method of testing of film is following under the normal temperature: choosing energy density is the laser irradiation testing sample of 1～50J/cm2; Measure 10 points with the mode of 1-on-1; Draw the probability of damage; Change its energy density then; Obtain the damage probability under the different-energy density laser; Choose 10 energy probability, promptly measure 10 * 10 points altogether; By computer the laser energy density that at every turn acts on the sample is gathered in real time; According to the damage probability in each energy density section, the laser energy density when drawing the zero probability damage by the linear fit method of mapping is the instant damage threshold of laser irradiation sample under the normal temperature then; Adopt the step pretreatment mode; Detailed process is: the preliminary treatment energy to every of film surface begins from 30% of normal temperature laser damage threshold; Increase by 10% then at every turn; Step is energization gradually; Stop up to increasing to 80%; Begin the preliminary treatment of next point then, film surface is all handled always;
Four, pretreated tantalum-oxide film is carried out anneal in atmosphere, annealing temperature is 200～400 ℃, and temperature rise rate is 0.01～20 ℃/min, and soaking time is 1～50h.
2. have the preparation method of high laser damage threshold tantalum oxide film under the hot environment according to claim 1, it is characterized in that: described substrate is BK7 glass or quartz.
3. the preparation method who has high laser damage threshold tantalum oxide film under the hot environment according to claim 1; It is characterized in that: described scavenging solution is any in sherwood oil, the acetone or alcohol; Or wherein any two kinds of described sherwood oil, acetone and ethanol, with the mixture of arbitrary volume ratio.
4. have the preparation method of high laser damage threshold tantalum oxide film under the hot environment according to claim 1, it is characterized in that: described annealing atmosphere be oxygen, nitrogen, argon gas or airborne any.
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| CN108445046A (en) * | 2018-01-24 | 2018-08-24 | 四川大学 | The comparative approach of resisting laser damage ability based on thin dielectric film capacitance characteristic |
| CN109115684A (en) * | 2018-09-07 | 2019-01-01 | 中国工程物理研究院激光聚变研究中心 | For determining the measurement method and measuring system of laser pre-treated energy level |
| CN110330236A (en) * | 2019-07-16 | 2019-10-15 | 中国矿业大学 | A kind of high temperature oxidation resisting niobium pentoxide film preparation method with high laser damage threshold |
| CN110330236B (en) * | 2019-07-16 | 2021-08-31 | 中国矿业大学 | Preparation method of high-temperature-resistant niobium oxide film with high laser damage threshold |
| CN110530206A (en) * | 2019-10-11 | 2019-12-03 | 河南平原光电有限公司 | High damage threshold protective film preparation process for laser intelligence field optics code-disc |
| CN112981353A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for eliminating film stress |
| CN112267098A (en) * | 2020-09-07 | 2021-01-26 | 中国科学院上海光学精密机械研究所 | Preparation method of space laser film |
| CN112267098B (en) * | 2020-09-07 | 2022-03-08 | 中国科学院上海光学精密机械研究所 | Preparation method of space laser film |
| CN112095081A (en) * | 2020-09-10 | 2020-12-18 | 天津津航技术物理研究所 | Preparation method of ultralow-stress high-reflection film |
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