CN210119589U - Picosecond laser high-power antireflection film - Google Patents
Picosecond laser high-power antireflection film Download PDFInfo
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- CN210119589U CN210119589U CN201920499410.3U CN201920499410U CN210119589U CN 210119589 U CN210119589 U CN 210119589U CN 201920499410 U CN201920499410 U CN 201920499410U CN 210119589 U CN210119589 U CN 210119589U
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Abstract
The utility model discloses a picosecond laser high power antireflection coating, including the stratum basale, the deposit has Hf layer and SiO layer in turn on the stratum basale2The number of layers of the Hf layer and the SiO2 layer was equal. The picosecond laser high-power antireflection film has the advantages that through the improvement of the film material and the structure, the transmittance at 1064 wave band can reach more than 99.8%, the transmittance at 650 wave band can reach more than 98%, the picosecond laser high-power antireflection film has higher laser damage threshold, simultaneously has high wear resistance and high adhesive force, has good stability, and can meet high-end application in the field of laser at present; the preparation repeatability is good, and the process is simple, easy to operate and control.
Description
Technical Field
The utility model relates to a picosecond laser high power antireflection coating belongs to picosecond laser antireflection coating field.
Background
The picosecond laser is a laser with picosecond pulse width, has the characteristics of picosecond-level ultrashort pulse width, adjustable repetition frequency, high pulse energy and the like, has increasingly wide application in the fields of biomedicine, optical parametric oscillation, biological microscopic imaging and the like, and gradually becomes an increasingly important tool in a modern biological imaging and analyzing system.
In an optical element, light energy is lost due to reflection on the surface of the element, and in order to reduce the reflection loss on the surface of the element, a transparent dielectric film is often coated on the surface of the optical element, and such a film is called an antireflection film.
The existing antireflection film is frequently applied to picosecond laser, and has the conditions of easy film burning, low durability and low laser damage resistance threshold.
SUMMERY OF THE UTILITY MODEL
The utility model provides a picosecond laser high power antireflection coating through the rational selection to the coating material and the rational design of structure for the rete that arrives has not only good spectral performance but also better mechanical stability ability and stability.
For solving the technical problem, the utility model discloses the technical scheme who adopts as follows:
a picosecond laser high-power antireflection film comprises a substrate layer, wherein Hf layers and SiO layers are alternately deposited on the substrate layer2The number of layers of the Hf layer and the SiO2 layer was equal.
The Hf is hafnium.
The applicant finds that the film absorbs laser energy to generate a thermal effect, so that the temperature of the film is increased, the film is heated rapidly in a short time,thermoelastic pressure and stress waves are generated around the local hot spot to intensify the final damage of the film; therefore, a material with small absorption must be selected to reduce the influence of the heat effect; the material with low refractive index is SiO2(the refractive index is 1.46), the film layer structure is amorphous, the dispersion is small at the working wavelength, the small optical coefficient is low, the absorption is small, and the laser damage threshold is high; the high refractive index material being TiO2、ZrO2And HfO2，TiO2The ZrO material is extremely easy to decompose in the heating evaporation process of an electron gun to generate low-order oxides, so that the absorption of a film layer is obviously increased, the evaporation rate of the ZrO material is unstable in the deposition process, large particles are easily formed, the refractive index is unstable, and the scattering loss is increased; HfO2The threshold value is higher, the absorption is less, but the hafnium metal is easy to splash during evaporation, and the method of evaporation of the hafnium metal which is not easy to splash in an oxygen environment is adopted, namely the hafnium metal has HfO2The good performance of the paint can avoid the defect of easy splashing.
The substrate layer is preferably a quartz glass substrate layer. The thickness of the substrate layer is preferably 2 ± 0.2 mm.
The application provides a high-power laser antireflection film with high laser damage threshold in visible light and near infrared double-waveband evaporation coating on the surface of a quartz substrate, the transmittance of the antireflection film in 1064 waveband can reach more than 99.8%, the transmittance in 650 waveband can reach more than 98%, the antireflection film has a high laser damage threshold, and the high-power laser antireflection film can meet high-end applications in the laser field at present; and the mechanical property is good and the stability is strong.
In order to take the spectral performance, the mechanical performance and the cost of the antireflection film into consideration, the number of the Hf layers and the SiO2 layers is preferably 2-5.
Preferably, the number of the f layers and the SiO2 layers is 2, that is, the picosecond laser high-power antireflection film comprises a substrate layer, and a first Hf layer, a first SiO2 layer, a second Hf layer and a second SiO2 layer are sequentially deposited on the substrate layer.
In order to take both the spectral performance and the mechanical performance of the antireflection film into consideration, the thickness of the first Hf layer is preferably smaller than that of the second Hf layer; the thickness of the first SiO2 layer is greater than that of the second SiO2 layer; the thickness of the first Hf layer is less than that of the second SiO2 layer, and the thickness of the second Hf layer is between that of the second SiO2 layer and that of the first SiO2 layer. Therefore, the mutual stress complementation effect of the films is good, and the spectral performance and the mechanical performance can be better guaranteed. The thickness of the present application is not particularly limited, and refers to physical thickness.
Preferably, the first SiO2The thickness of the layer is 7-8 times of the thickness of the first Hf layer, the thickness of the second Hf layer is 3.5-4 times of the first Hf layer, and the second SiO layer2The thickness of the layer is 3-3.4 times the thickness of the first Hf layer. Therefore, the spectral performance and the mechanical performance of the antireflection film can be better guaranteed.
In order to take both the spectral performance and the mechanical performance of the antireflection film into consideration, it is further preferable that the thickness of the first Hf layer is 319.2 ± 10nm, the thickness of the first SiO2 layer is 2447.2 ± 10nm, the thickness of the second Hf layer is 1170.4 ± 10nm, and the thickness of the second SiO2 layer is 1032.08 ± 10 nm.
That is, the preferred film layer structure is designed to: SUB/k1Hk2Lk3Hk4L/A, wherein SUB represents JGS1 substrate, A represents air, H represents Hf, and L represents SiO2(ii) a k1-k4 represent the coefficients for the quarter-reference wavelength (1064nm) optical thickness of each layer, 0.3/2.3/1.1/0.97, respectively.
According to the preparation method of the picosecond laser high-power antireflection film, an Hf layer and an SiO2 layer are sequentially and alternately deposited on a substrate layer by adopting an ion source assisted electron beam evaporation method.
In order to ensure the spectral performance and the mechanical performance of the antireflection film, the preparation method of the picosecond laser high-power antireflection film comprises the following steps:
1) for hafnium and SiO2Performing independent pre-melting treatment on the membrane material to remove impurities in the membrane material;
2) cleaning the substrate layer, placing in a vacuum chamber under pressure of (1.8 + -0.2) x 10-3Under the conditions of Pa and the baking temperature of 250-300 ℃, an ion source assisted electron beam evaporation method is adopted to sequentially deposit a composite layer and MgF on the surface of the substrate layer2And (3) a layer.
In order to improve the adhesion of the film, in step 2), the base layer cleaning method comprises the following steps: and performing ultra-smooth surface polishing on the surface of the base layer to ensure that the surface roughness Ra is less than 5 angstroms, and performing ultrasonic cleaning on the surface of the substrate before film coating to remove microscopic particles attached to the surface of the substrate so as to ensure that the adhesiveness of the film layer is stronger.
In order to improve the quality of the film, in the step 2), during deposition, high-purity oxygen (more than or equal to 99.99 percent) with stronger oxidation capacity than that of common molecular oxygen is introduced into the vacuum chamber, so that the deposition material can be fully oxidized in a high vacuum state, the film forming compactness is improved under the action of a radio frequency source, the absorption of the film is reduced, and the laser damage resistance threshold is improved. The method not only retains the unique favorable performance of the laser film prepared by the electron beam thermal evaporation method, but also improves the intrinsic absorption and defect density of the film, and has the characteristics of strong pertinence, high quality, simplicity and feasibility.
Further preferably, when the Hf layer is deposited, the gas filling amount of the high-purity oxygen is 150-; deposition of Hf layer SiO2When the oxygen is used, the aeration quantity of the high-purity oxygen is 60-100 sccm.
Preferably, the ion source beam current is 20A.
In order to ensure the film quality, it is preferable that the evaporation rate of Hf is 0.15. + -. 0.02nm/S, SiO2The evaporation rate of (3) is 1. + -. 0.02 nm/S.
The technology not mentioned in the present invention refers to the prior art.
The picosecond laser high-power antireflection film has the advantages that through the improvement of the film material and the structure, the transmittance at 1064 wave band can reach more than 99.8%, the transmittance at 650 wave band can reach more than 98%, the picosecond laser high-power antireflection film has higher laser damage threshold, simultaneously has high wear resistance and high adhesive force, has good stability, and can meet high-end application in the field of laser at present; the preparation repeatability is good, and the process is simple, easy to operate and control.
Drawings
FIG. 1 is a schematic view of the structure of a picosecond laser high power antireflection film of example 1 (the substrate layer is omitted in the figure);
FIG. 2 is a graph showing the double-sided transmittance design curve of the picosecond laser high-power antireflection film in example 1;
FIG. 3 is a plot of the single-sided reflectivity design for the picosecond laser high power antireflective film of example 1;
FIG. 4 is a graph of the measured spectrum of the picosecond laser high power antireflection film of example 1 (a is the double-sided transmittance and b is the single-sided reflectance);
in the figure, 1 is the base layer side, 2 is the first Hf layer, and 3 is the first SiO2Layer, 4 is a second Hf layer, 5 is a second SiO2Layer 6 is the air side.
Detailed Description
For a better understanding of the present invention, the following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples.
The coating equipment is selected from a Japanese Showa coating machine (SGC-S1300Ci), and is provided with a double condensation pump (ULVAC RBH-22), a Polycold (PFC-1102HC), a double electron gun (Nisshin technology research NEB-10WE type) and a radio frequency ion source (SER. NO 12-4088);
example 1
As shown in FIG. 1, the picosecond laser high-power antireflection film comprises a substrate layer, wherein a first Hf layer and a first SiO layer are sequentially deposited on the substrate layer2Layer, second Hf layer and second SiO2The basal layer is a quartz glass basal layer with the thickness of 2 mm.
The thickness of the first Hf layer was 319.2nm, the first SiO2The thickness of the layer was 2447.2nm, the thickness of the second Hf layer was 1170.4nm, the second SiO2The thickness of the layer was 1032.08 nm.
The preparation method of the picosecond laser high-power antireflection film comprises the following steps:
1) for hafnium and SiO2Performing independent pre-melting treatment on the membrane material to remove impurities in the membrane material;
2) performing ultra-smooth surface polishing on the surface of the substrate layer to make the surface roughness Ra less than 5 angstroms, ultrasonic cleaning, and placing in a vacuum chamber with pressure of 1.8 × 10-3Under the conditions of Pa and the baking temperature of 280 ℃, an ion source assisted electron beam evaporation method is adopted to sequentially deposit a composite layer and MgF on the surface of the substrate layer2During deposition, high-purity oxygen is introduced into the vacuum chamber to fully oxidize the deposited material in high vacuum state, and under the action of the radio frequency source, the film forming compactness is improved, the absorption of the film is reduced, and the laser damage resistance threshold is improvedThe value is that when the Hf layer is deposited, the gas filling amount of the high-purity oxygen is 150-; deposition of Hf layer SiO2Meanwhile, the gas filling amount of the high-purity oxygen is 60-100sccm, and the ion source beam current is 20A; the evaporation rate of Hf is 0.15nm/S, SiO2The evaporation rate of (3) was 1 nm/S. By adding the isolation baffle between the evaporation source and the substrate layer, invalid evaporation materials are blocked and adsorbed, pollution near the substrate layer is reduced, and the probability of forming film defects is reduced.
The single-sided reflectivity and the double-sided transmittance of the antireflection film of the example were measured by using a PHOTO RT spectrophotometer in white russia, and the obtained spectral curve meets the design requirements, as shown in fig. 4, and fig. 2 to 3 are design curves.
The highest laser damage threshold of the existing PVD coating can reach 28.4J/cm2(laser pulse width 10ns, 1-on-1 detection mode), and the actual measurement result of the antireflection film of this example is 40J/cm2(detection by Spica Technologies inc., usa); in the antireflection film of this example, the laser damage threshold at a repetition frequency of 10KHZ with a laser having a pulse width of 6ps and a wavelength of 1064nm was 12J/cm2。
Example 2
A picosecond laser high-power antireflection film comprises a substrate layer, wherein a first Hf layer and a first SiO layer are sequentially deposited on the substrate layer2Layer, second Hf layer and second SiO2The basal layer is a quartz glass basal layer with the thickness of 2 mm. The thickness of the first Hf layer was 320.5nm, the first SiO2The thickness of the layer was 2450.3nm, the thickness of the second Hf layer was 1172.6nm, the second SiO2The thickness of the layer was 1030.8 nm.
The preparation method of the picosecond laser high-power antireflection film refers to example 1. In the antireflection film of this example, the laser damage threshold at a repetition frequency of 10KHZ with a laser having a pulse width of 6ps and a wavelength of 1064nm was 12J/cm2。
The films obtained in the above examples are subjected to the following environmental tests according to the requirements of the general specification of GJB2485-95 optical film layers:
(1) abrasion resistance test: wrapping 2 layers of dry absorbent gauze outside the rubber friction head, and rubbing the film layer along the same track under the pressure of 4.9N for 25 times without damage such as scratches.
(2) Adhesion force experiment: the adhesive tape with the width of 2cm and the peel strength I of more than 2.94N/cm is firmly adhered to the surface of the film layer, and after the adhesive tape is quickly pulled up from the edge of the part to the vertical direction of the surface, the film layer does not fall off and is not damaged.
(3) Soaking test: and completely immersing the sample into distilled water or deionized water, wherein the film layer does not have the defects of new peeling, cracks, foaming and the like after 96 hours.
And (4) conclusion: the ultrasonic-assisted cleaning technology is adopted in each example, and the obtained film layer has good spectral performance and good mechanical stability and stability through reasonable selection and design of the film material.
Claims (10)
1. A picosecond laser high-power antireflection film is characterized in that: comprises a substrate layer on which Hf and SiO layers are alternately deposited2Layer, Hf layer and SiO2The number of layers is equal.
2. The picosecond laser high power antireflective film of claim 1, wherein: hf layer and SiO2The number of layers is 2-5.
3. The picosecond laser high power antireflective film of claim 1 or 2, wherein: comprises a substrate layer, a first Hf layer and a first SiO layer are deposited on the substrate layer in sequence2Layer, second Hf layer and second SiO2And (3) a layer.
4. The picosecond laser high power antireflective film of claim 3, wherein: the thickness of the first Hf layer is less than that of the second Hf layer; the thickness of the first SiO2 layer is greater than the thickness of the second SiO2 layer.
5. The picosecond laser high power antireflective film of claim 4, wherein: the thickness of the first Hf layer is less than that of the second SiO2 layer, and the thickness of the second Hf layer is between that of the second SiO2 layer and that of the first SiO2 layer.
6. The picosecond laser high power antireflective film of claim 5, wherein: first SiO2The thickness of the layer is 7-8 times of the thickness of the first Hf layer, the thickness of the second Hf layer is 3.5-4 times of the first Hf layer, and the second SiO layer2The thickness of the layer is 3-3.4 times the thickness of the first Hf layer.
7. The picosecond laser high power antireflective film of claim 6, wherein: the thickness of the first Hf layer is 319.2 +/-10 nm, and the first SiO layer2The thickness of the layer is 2447.2 + -10 nm, the thickness of the second Hf layer is 1170.4 + -10 nm, the second SiO layer2The thickness of the layer was 1032.08 + -10 nm.
8. The picosecond laser high power antireflective film of claim 1 or 2, wherein: the substrate layer is a quartz glass substrate layer.
9. The picosecond laser high power antireflective film of claim 1 or 2, wherein: the thickness of the substrate layer is 2 +/-0.2 mm.
10. The picosecond laser high power antireflective film of claim 1 or 2, wherein: the transmittance in 1064 band is 99.8% or more, and the transmittance in 650 band is 98% or more.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110007377A (en) * | 2019-04-15 | 2019-07-12 | 南京波长光电科技股份有限公司 | A kind of picosecond laser high power anti-reflection film and preparation method thereof |
| CN113684449A (en) * | 2021-08-06 | 2021-11-23 | 南京波长光电科技股份有限公司 | Low-absorption high-power optical fiber laser antireflection film and preparation method thereof |
| CN110007377B (en) * | 2019-04-15 | 2024-06-21 | 南京波长光电科技股份有限公司 | Picosecond laser high-power antireflection film and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110007377A (en) * | 2019-04-15 | 2019-07-12 | 南京波长光电科技股份有限公司 | A kind of picosecond laser high power anti-reflection film and preparation method thereof |
| CN110007377B (en) * | 2019-04-15 | 2024-06-21 | 南京波长光电科技股份有限公司 | Picosecond laser high-power antireflection film and preparation method thereof |
| CN113684449A (en) * | 2021-08-06 | 2021-11-23 | 南京波长光电科技股份有限公司 | Low-absorption high-power optical fiber laser antireflection film and preparation method thereof |
| CN113684449B (en) * | 2021-08-06 | 2023-09-08 | 南京波长光电科技股份有限公司 | Low-absorption high-power optical fiber laser antireflection film and preparation method thereof |
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