CN209842108U - Three-band laser antireflection film - Google Patents

Three-band laser antireflection film Download PDF

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CN209842108U
CN209842108U CN201920499480.9U CN201920499480U CN209842108U CN 209842108 U CN209842108 U CN 209842108U CN 201920499480 U CN201920499480 U CN 201920499480U CN 209842108 U CN209842108 U CN 209842108U
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layer
thickness
znse
antireflection film
band laser
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李全民
陈佳佳
朱敏
吴玉堂
王国力
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Nanjing Wavelength Optoelectronics Technology Co Ltd
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Nanjing Wavelength Optoelectronics Technology Co Ltd
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Abstract

The utility model discloses a three wave band laser antireflection coating, including the stratum basale, deposit in proper order on the stratum basale has composite bed and MgF2A layer; the composite layer includes alternately deposited YF3A layer and a ZnSe layer, wherein the base layer is connected with the YF3Layer by layer,MgF2The layer is connected with the ZnSe layer. The utility model discloses three wave band laser antireflection coatings, 650nm wave band's single face reflectivity is less than or equal to 1%, 1570nm wave band's single face reflectivity is less than or equal to 0.25%, 10.6 mu m wave band's single face reflectivity<0.25 percent, meets the use requirements of an optical system of multi-wavelength laser processing equipment, has excellent optical performance, strong film adhesion, strong friction resistance, good water resistance and temperature resistance, good spectral performance and good mechanical stability and stability; the preparation repeatability is good, and the process is simple, easy to operate and control.

Description

Three-band laser antireflection film
Technical Field
The utility model relates to a three wave band laser antireflection coating belongs to three wave band laser antireflection coating field.
Background
The modern visible/near infrared spectrum analysis technology can fully utilize full-spectrum or multi-wavelength spectrum data for analysis, has the characteristics of large information amount, high speed, good reproducibility, convenient measurement and the like, and is widely applied to the fields of food, agriculture, chemical industry, pharmacy and the like.
In modern optical systems, most optical components need to be coated with antireflection films to reduce surface reflection, especially for use in special environments to optical systems, and in addition to requiring higher optical performance of the films, the films also need to be resistant to various harsh environments.
However, the existing antireflection film has the problems of easy delamination, peeling, poor adhesion and the like, and no related report of the three-band laser antireflection film exists at present.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems of film layering, peeling and poor adhesive force, the obtained film has both good spectral performance and better mechanical stability and stability, the utility model provides a 10.6 mu m &1570nm &650nm three-band laser antireflection film.
For solving the technical problem, the utility model discloses the technical scheme who adopts as follows:
a three-band laser antireflection film comprises a substrate layer, wherein a composite layer and MgF are sequentially deposited on the substrate layer2A layer; the composite layer includes alternately deposited YF3A layer and a ZnSe layer, wherein the base layer is connected with the YF3Layers being joined to each other, MgF2The layer is connected with the ZnSe layer.
The applicant finds that YF3The film material has low refractive index, wide light transmission range from visible light to 14 mu m, good optical property and process property, and is a very suitable low-refractive index material; in addition, the MgF2 has high hardness, good mechanical property, stable chemical property, difficult deliquescence and corrosion, and the optical property is mainly characterized in that the MgF2 has lower absorption in a vacuum visible light wave band, so that the MgF2 is used as the outermost layer, the transmittance of the film can be improved, and the film layer can be more resistant to friction; YF with specific structure3、ZnSe、MgF2The combination of the three coating materials ensures that the single-side reflectivity of the antireflection film at 650nm wave band is less than or equal to 1 percent, the single-side reflectivity at 1570nm wave band is less than or equal to 0.25 percent, and the single-side reflectivity at 10.6 mu m wave band<0.25 percent, meets the use requirements of an optical system of multi-wavelength laser processing equipment, and has strong film adhesion, strong friction resistance, strong water resistance, good temperature resistance, good spectral performance, good mechanical stability and stability.
For further improving the mechanical property and optical property of the antireflection film, YF is preferable3The number of layers is equal to that of the ZnSe layer, and the ZnSe layer is 4-6.
Further preferably, YF3The number of layers and the number of layers of ZnSe are both 5, namely the three-band laser antireflection film comprises a substrate layer, and a first YF is sequentially deposited on the substrate layer3Layer, first ZnSe layer, second YF3Layer, second ZnSe layer, third YF3Layer, third ZnSe layer, fourth YF3Layer, fourth ZnSe layer, fifth YF3Layer, fifth ZnSe layer and MgF2And (3) a layer.
In order to give consideration to both the mechanical property and the optical property of the antireflection film, the first YF is preferable3The thickness of the layer is less than the second YF3Thickness of layer, second YF3The thickness of the layer is less than the third YF3Thickness of layer, fourth YF3The thickness of the layer is between the first YF3Thickness of layer and second YF3Between the thickness of the layers, fifth YF3The thickness of the layer is less than the first YF3The thickness of the layer; the thickness of the first ZnSe layer is greater than that of the second ZnSe layer, and the thickness of the third ZnSe layer is greater than that of the third ZnSe layerThe thickness of the first ZnSe layer is larger than that of the second ZnSe layer, the thickness of the fourth ZnSe layer is larger than that of the first ZnSe layer, the thickness of the fifth ZnSe layer is larger than that of the second ZnSe layer, and the thickness of the MgF layer is larger than that of the first ZnSe layer2The thickness of the layer is larger than that of the fifth ZnSe layer, so that the mutual stress complementation effect of the film layers is good, and the mechanical property and the spectral property of the antireflection film can be better ensured. The thickness of the present application is not particularly limited, and refers to physical thickness.
To further enhance the complementary effect between the film layers, a third YF3The thickness of the layer is fifth YF325-30 times the thickness of the layer; the thickness of the third ZnSe layer is 5-6 times of that of the second ZnSe layer; third YF3The thickness of the layer is 3-4 times of the thickness of the third ZnSe layer; MgF2The thickness of the layer is 1.8-2.2 times the thickness of the fifth ZnSe layer.
In order to meet the requirements of cost and product quality, the first YF is preferably selected3The thickness of the layer is 204 +/-10 nm, the thickness of the first ZnSe layer is 420 +/-10 nm, and the second YF3The thickness of the layer is 390 plus or minus 10nm, the thickness of the second ZnSe layer is 270 plus or minus 10nm, and the third YF3The thickness of the layer is 5328 +/-10 nm, the thickness of the third ZnSe layer is 1500 +/-10 nm, and the fourth YF3The thickness of the layer is 246 + -10 nm, the thickness of the fourth ZnSe layer is 486 + -10 nm, and the fifth YF3The thickness of the layer is 192 +/-10 nm, the thickness of the fifth ZnSe layer is 342 +/-10 nm, and MgF2The thickness of the layer was 690. + -.10 nm.
In the above structure, the first 10 YF layers on the base layer3The two coating materials of ZnSe are alternately used, and MgF is used as the outermost layer2And generating a structure: SUB/aNbHcNdHefHgNhHiNjHkM/A, wherein SUB represents a substrate layer, A represents air, and N represents YF3Layer, M represents MgF2Layer, H represents a ZnSe layer; a-k represent the coefficients of the quarter-reference wavelength (600nm) optical thickness of each layer, respectively: 0.34,0.70,0.65,0.45,8.88,2.50,0.41,0.81,0.32,0.57,1.15.
The commonly used high-refractive-index materials in the infrared band comprise ZnSe and ZnS, and preferably, the substrate layer is a ZnSe substrate layer. The film system has small absorption to light with wavelength of 10.6 microns, ZnSe light transmission range of 0.5-15 microns, extremely low scattering loss and high thermal shock bearing capacity, so the film system is a preferred material for manufacturing an infrared high-power laser film system. Preferably, the thickness of the base layer is 2. + -. 0.2 mm.
According to the three-band laser antireflection film, a composite layer and MgF are sequentially deposited on a substrate layer in a vacuum evaporation mode2And (3) a layer.
The preparation method of the three-band laser antireflection film comprises the following steps:
1) for YF3、ZnSe、MgF2Performing 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 10-3Sequentially depositing a composite layer and MgF on the surface of the substrate layer under the conditions of Pa and the baking temperature of 100 +/-5 DEG C2And (3) a layer.
In order to improve the bonding force between the film layers and the adhesive force of the film layers, in the step 2), a Koufman ion-assisted deposition composite layer and MgF are adopted2And (3) a layer. The applicant has found that this increases the packing density, improves structural integrity and stress matching, and thus improves the performance and lifetime of the membrane layer,
the ion source beam current for ion assisted deposition is preferably 20A. The ion-assisted deposition is adopted in the film coating process, so that the problem of stress between film layers is effectively solved, the compactness of the film layers is improved, the film layers are firmer, and the service life is longer.
In order to further improve the adhesion of the film layer, the substrate layer is cleaned by adopting an ion bombardment method in the step 2). The applicant has found that this increases the coagulation coefficient and enhances the adhesion of the film.
The optical control method is adopted to control the optical thickness, the crystal control method is adopted to control the evaporation rate, the evaporation rate of YF3 is controlled to be 0.4 +/-0.02 nm/s, and the evaporation rates of ZnS and MgF2 are respectively controlled to be 0.25 +/-0.02 nm/s and 0.7 +/-0.02 nm/s.
The utility model provides a surface coating by vaporization at zinc selenide has included the antireflection coating of visible light, near-infrared and the three wave band of long wave infrared structure and preparation method, through ion-assisted deposition, adjustment process parameter, obtained optical property is good, the preparation repeatability is good, the rete adhesive force is strong, three wave band antireflection coating of antifriction, this antireflection coating is less than or equal to 1% at the single face reflectivity of 650nm wave band, the single face reflectivity of 1570nm wave band is less than or equal to 0.25%, the single face reflectivity of 10.6 mu m wave band < 0.25%, satisfied multi-wavelength laser processing equipment optical system's operation requirement.
The technology not mentioned in the present invention refers to the prior art.
The utility model discloses three wave band laser antireflection coatings, 650nm wave band's single face reflectivity is less than or equal to 1%, 1570nm wave band's single face reflectivity is less than or equal to 0.25%, 10.6 mu m wave band's single face reflectivity < 0.25%, satisfied multi-wavelength laser processing equipment optical system's operation requirement, optical property is good, and the rete adhesive force is strong, and the antifriction is strong, and water proofness and temperature tolerance are good, and not only good spectral performance has better mechanical stability ability and stability again; the preparation repeatability is good, and the process is simple, easy to operate and control.
Drawings
FIG. 1 is a schematic view showing the structure of a three-band laser antireflection film according to example 1 (the base layer is omitted);
FIG. 2 is a single-sided reflection curve (wavelength nm in abscissa and reflectance in ordinate) of the three-band laser antireflection film of example 1 at 650nm and 1570nm bands;
FIG. 3 is a single-sided reflection curve (wavelength nm in abscissa and reflectance in ordinate) of the three-band laser antireflection film in example 1 at a band of 10.6 μm;
FIG. 4 is a graph showing the double-sided transmission curves of the three-band laser antireflection film of example 1 at 650nm and 1570nm (wavelength nm on the abscissa and transmittance on the ordinate);
FIG. 5 is a graph showing a double-sided transmission curve (wavelength nm in abscissa and transmittance in ordinate) of the three-band laser antireflection film of example 1 at a wavelength of 10.6 μm;
in the figure, a is the first YF3Layer, b is a first ZnSe layer, c is a second YF3Layer, d is a second ZnSe layer, e is a third YF3Layer, f is a third ZnSe layer, g is a fourth YF3Layer, h is the fourth ZnSe layer, i is the fifth YF3A layer of a material selected from the group consisting of,j is a fifth ZnSe layer, k is MgF2A layer; the base layer is a ZnSe base layer, 1 is the base layer side, and 2 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.
In the following example, a Nanguang 800 type film coating machine is adopted, an INFICON SQC-310 controller is adopted for crystal control, and the quality and thickness of the film are measured by using the oscillation frequency change of a quartz crystal. The ion source adopts a Koffman ion source developed in the nine kingdoms of China, and the density of a deposited film can be improved and the optical and mechanical properties can be improved by reasonably controlling the ion energy. The vacuum chamber is matched with a diffusion pump system through a mechanical pump to obtain the vacuum degree required by the experiment, and the vacuum degree is measured through a thermocouple meter.
Example 1
As shown in FIG. 1, a three-band laser antireflection film comprises a substrate layer, wherein a first YF is sequentially deposited on the substrate layer3Layer, first ZnSe layer, second YF3Layer, second ZnSe layer, third YF3Layer, third ZnSe layer, fourth YF3Layer, fourth ZnSe layer, fifth YF3Layer, fifth ZnSe layer and MgF2A layer; the substrate layer is a ZnSe substrate layer.
The thickness of the ZNSE substrate layer is 2mm, and the first YF3The thickness of the layer is 204nm, the thickness of the first ZnSe layer is 420nm, and the second YF3The thickness of the layer is 390nm, the thickness of the second ZnSe layer is 270nm, and the third YF3The thickness of the layer is 5328nm, the thickness of the third ZnSe layer is 1500nm, and the fourth YF3The thickness of the layer was 246nm, the thickness of the fourth ZnSe layer was 486nm, the fifth YF3The thickness of the layer was 192nm, the thickness of the fifth ZnSe layer was 342nm, MgF2The thickness of the layer was 690 nm.
The preparation method of the three-band laser antireflection film comprises the following steps of:
1) for YF3ZnSe and MgF2Performing independent pre-melting treatment on the membrane material to remove impurities in the membrane material;
2) before coating, the substrate is ion bombarded for 5min to clean substrate, raise coagulation coefficient and strengthen adhesion of film layer, and the substrate is set inside vacuum chamber with pressure of 1.8 × 10-3Under the conditions of Pa and the baking temperature of 100 ℃, a composite layer and MgF are sequentially deposited on the surface of the substrate layer2The layer, at the sedimentary in-process of rete, uses the auxiliary deposit of koffman ion source, increases the gathering density, improves structural integrity and stress matching to improved the performance and the live time of rete, adopted light-operated method control optics thickness, adopted the crystal control method to control evaporation rate simultaneously, the ion source parameter sets up to: accelerating voltage of 250V, screen electrode voltage of 400V, beam current of 20mA, YF3The evaporation rate of the ZnS is controlled to be 0.25nm/s, the evaporation rate of the ZnS is controlled to be 0.4nm/s, and MgF2The evaporation rate of (2) was controlled at 0.7 nm/s.
The single-sided reflectivity and the double-sided transmittance of the projection-enhanced film were measured by using a PHOTO RT spectrophotometer of russia and a Spectrum100 infrared spectrometer of PE corporation of america, and the obtained spectral curve reached the design requirements, as shown in fig. 2 to 5.
Example 2
A three-band laser antireflection film comprises a substrate layer, a first YF layer and a second YF layer sequentially deposited on the substrate layer3Layer, first ZnSe layer, second YF3Layer, second ZnSe layer, third YF3Layer, third ZnSe layer, fourth YF3Layer, fourth ZnSe layer, fifth YF3Layer, fifth ZnSe layer and MgF2A layer; the substrate layer is a ZnSe substrate layer.
The thickness of the ZNSE substrate layer is 2mm, and the first YF3The thickness of the layer is 206nm, the thickness of the first ZnSe layer is 423nm, and the second YF3The thickness of the layer was 394nm, the thickness of the second ZnSe layer was 265nm, and the third YF3The thickness of the layer is 5325nm, the thickness of the third ZnSe layer is 1502nm, and the fourth YF3The thickness of the layer is 249nm, the thickness of the fourth ZnSe layer is 488nm, and the thickness of the fifth YF3The thickness of the layer was 195nm, the thickness of the fifth ZnSe layer was 345nm, MgF2The thickness of the layer was 692 nm.
The films obtained in the above examples were 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 40 times without damage such as scratches.
(2) Adhesion force experiment: and (3) adhering a 3M adhesive tape with the width of 1cm to the surface of the film layer firmly, and quickly pulling up the adhesive tape from the edge of the part to the vertical direction of the surface, wherein the film layer is not fallen off and damaged.
(3) Soaking test: the sample is completely immersed in distilled water or deionized water, and no abnormality occurs in the membrane layer after 96 hours.
(4) High-temperature test: heating to 150 deg.C from normal temperature, baking for 1 hr, cooling to normal temperature, and repeating twice until no film layer is abnormal.
The utility model discloses a reasonable selection of coating material adopts the supplementary deposition technique of ion beam, solves stress and rete adhesive force between the rete, makes the rete that obtains have good spectral performance but also have better mechanical stability ability and stability.

Claims (10)

1. A three-band laser antireflection film is characterized in that: comprises a substrate layer, wherein a composite layer and MgF are deposited on the substrate layer in sequence2A layer; the composite layer includes alternately deposited YF3A layer and a ZnSe layer, wherein the base layer is connected with the YF3Layers being joined to each other, MgF2The layer is connected with the ZnSe layer.
2. The three-band laser antireflection film of claim 1 wherein: YF3The number of layers is equal to that of the ZnSe layer, and the ZnSe layer is 4-6.
3. The three-band laser antireflection film of claim 2 wherein: comprises a substrate layer, on which a first YF is sequentially deposited3Layer, first ZnSe layer, second YF3Layer, second ZnSe layer, third YF3Layer, third ZnSe layer, fourth YF3Layer, fourth ZnSe layer, fifth YF3Layer, fifth ZnSe layer and MgF2And (3) a layer.
4. The three-band laser antireflection film of claim 3 wherein: first YF3The thickness of the layer is less than the second YF3Thickness of layer, second YF3The thickness of the layer is less than the third YF3Thickness of layer, fourth YF3The thickness of the layer is between the first YF3Thickness of layer and second YF3Between the thickness of the layers, fifth YF3The thickness of the layer is less than the first YF3The thickness of the layer.
5. The three-band laser antireflection film of claim 4 wherein: third YF3The thickness of the layer is fifth YF325-30 times the thickness of the layer.
6. The three-band laser antireflection film of claim 5 wherein: the thickness of the first ZnSe layer is larger than that of the second ZnSe layer, the thickness of the third ZnSe layer is larger than that of the first ZnSe layer, the thickness of the fourth ZnSe layer is between that of the first ZnSe layer and that of the third ZnSe layer, and the thickness of the fifth ZnSe layer is between that of the second ZnSe layer and that of the first ZnSe layer.
7. The three-band laser antireflection film of claim 6 wherein: the thickness of the third ZnSe layer is 5-6 times of the thickness of the second ZnSe layer.
8. The three-band laser antireflection film of claim 7 wherein: third YF3The thickness of the layer is 3-4 times of the thickness of the third ZnSe layer; MgF2The thickness of the layer is 1.8-2.2 times the thickness of the fifth ZnSe layer.
9. The three-band laser antireflection film of claim 8 wherein: first YF3The thickness of the layer is 204 +/-10 nm, the thickness of the first ZnSe layer is 420 +/-10 nm, and the second YF3The thickness of the layer is 390 plus or minus 10nm, the thickness of the second ZnSe layer is 270 plus or minus 10nm, and the third YF3The thickness of the layer is 5328 + -10 nmThe thickness of the three ZnSe layers is 1500 +/-10 nm, and the fourth YF layer3The thickness of the layer is 246 + -10 nm, the thickness of the fourth ZnSe layer is 486 + -10 nm, and the fifth YF3The thickness of the layer is 192 +/-10 nm, the thickness of the fifth ZnSe layer is 342 +/-10 nm, and MgF2The thickness of the layer was 690. + -.10 nm.
10. The three-band laser antireflection film of any one of claims 1 to 9 wherein: the substrate layer is a ZnSe substrate layer, and the thickness of the substrate layer is 2 +/-0.2 mm; the single-side reflectivity of the three-band laser antireflection film at 650nm is less than or equal to 1 percent, the single-side reflectivity at 1570nm is less than or equal to 0.25 percent, and the single-side reflectivity at 10.6 mu m is less than 0.25 percent.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109991691A (en) * 2019-04-15 2019-07-09 南京波长光电科技股份有限公司 Three wave band of laser anti-reflection films of one kind and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109991691A (en) * 2019-04-15 2019-07-09 南京波长光电科技股份有限公司 Three wave band of laser anti-reflection films of one kind and preparation method thereof
CN109991691B (en) * 2019-04-15 2024-01-05 南京波长光电科技股份有限公司 Three-band laser antireflection film and preparation method thereof

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