CN114236661A - Single crystal germanium infrared crystal spectroscope and preparation method of laser long-wave infrared beam splitting film - Google Patents
Single crystal germanium infrared crystal spectroscope and preparation method of laser long-wave infrared beam splitting film Download PDFInfo
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Abstract
The invention relates to a monocrystalline germanium infrared crystal spectroscope and a preparation method of a laser long-wave infrared beam splitting film, belonging to the technical field of optical film manufacturing; the spectroscope consists of a single crystal germanium infrared crystal substrate and a beam splitting film with high reflection at an incident angle of 45 degrees of 1.064 mu m and high transmittance of 7.7 mu m-10.3 mu m. The film system of the beam splitting film comprises 22 layers from inside to outside, wherein the film materials of the odd film layers are YbF3And the film materials of the even film layers are ZnS. The invention strictly executes the program to set the process parameters (geometric thickness, temperature, deposition rate and vacuum degree) of each layer of coating film, and controls the geometric thickness of the film layer by combining with the film layer thickness online control system, thus realizing the preparation of the laser long-wave infrared beam splitter film of the monocrystalline germanium infrared crystal beam splitter and finally achieving the required optical characteristic technical index.
Description
Technical Field
The invention belongs to the technical field of optical film manufacturing, and particularly relates to a monocrystalline germanium infrared crystal spectroscope and a preparation method of a laser long-wave infrared beam splitting film.
Background
The spectroscope is used as a key optical element of a 'multi-light-in-one' optical system, is widely applied to the interior of an optoelectronic system, can effectively realize light transmission and light energy distribution, and greatly simplifies the system structure. In order to meet the requirement that one part of energy of the light beam in the same path is reflected and the other part of the energy is transmitted, the optical performance is realized by adopting an optical coating technology. The single crystal germanium infrared crystal is a key element of an optical light splitting system product, and in order to improve the optical performance of the single crystal germanium infrared crystal, a 1.064 mu m and 7.7 mu m-10.3 mu m dual-band beam splitting film is required to be plated on the surface of a single crystal germanium infrared crystal substrate.
In the prior art, a film is coated by electron beam evaporation and can be matched with a quartz crystal control system and an optical film thickness control system for automatic film coating, beam splitting film systems are non-regular film systems, and system errors and random errors are inevitably introduced in the actual film coating process due to the influence of comprehensive factors of a film coating environment, so that a film spectrum curve actually prepared is different from a spectrum curve theoretically designed.
Disclosure of Invention
The technical problem to be solved is as follows:
in order to avoid the defects of the prior art, the invention provides a single-crystal germanium infrared crystal spectroscope and a preparation method of a laser long-wave infrared beam splitting film, wherein the single-crystal germanium infrared crystal spectroscope consists of a single-crystal germanium infrared crystal substrate and a beam splitting film with an incident angle of 45 degrees, high reflection at 1.064 mu m and high transmittance at 7.7-10.3 mu m.
The technical scheme of the invention is as follows: a single crystal germanium infrared crystal beamsplitter, comprising: the device comprises a substrate and a beam splitting film plated on the substrate, wherein the substrate is a single crystal germanium infrared crystal, and the beam splitting film is a laser long-wave infrared beam splitting film.
The further technical scheme of the invention is as follows: when the beam splitting film is incident at 45 degrees, the reflectivity test value of a 1.064 mu m laser waveband is 98.25%; the average value of the transmittance test of the long-wave infrared band with the wavelength of 7.7-10.3 mu m is 98.71 percent.
The further technical scheme of the invention is as follows: the film system of the laser long-wave infrared beam splitting film is arranged from inside to outsideComprises 22 layers, wherein the film materials of the odd film layers are YbF3And the film materials of the even film layers are ZnS.
The further technical scheme of the invention is as follows: the geometric thicknesses of the film system 22 layers are respectively as follows: layer 1 geometric thickness 145.28nm, layer 2 geometric thickness 437.03nm, layer 3 geometric thickness 50.00nm, layer 4 geometric thickness 416.83nm, layer 5 geometric thickness 196.36nm, layer 6 geometric thickness 97.66nm, layer 7 geometric thickness 278.71nm, layer 8 geometric thickness 54.03nm, layer 9 geometric thickness 311.65nm, layer 10 geometric thickness 50.60nm, layer 11 geometric thickness 288.91nm, layer 12 geometric thickness 86.06nm, layer 13 geometric thickness 223.21nm, layer 14 geometric thickness 129.89nm, layer 15 geometric thickness 158.52nm, layer 16 geometric thickness 632.23nm, layer 17 geometric thickness 171.26nm, layer 18 geometric thickness 129.94nm, layer 19 geometric thickness 644.37nm, layer 20 geometric thickness 50.00nm, layer 21 geometric thickness 682.16nm, layer 22 geometric thickness 91.16 nm.
A method for preparing a laser long-wave infrared beam splitting film of a monocrystalline germanium infrared crystal spectroscope is characterized by comprising the following specific steps:
the method comprises the following steps: plating a 1 st film layer: taking YbF3The film material is evaporated by a resistance evaporation source with the vacuum degree less than or equal to 1.0 multiplied by 10- 3Pa, evaporation rate of 0.8 nm/s-0.9 nm/s;
step two: plating a 2 nd layer film layer: taking ZnS film material to carry out evaporation by a resistance evaporation source, wherein the vacuum degree is less than or equal to 1.0 multiplied by 10- 3Pa, evaporation rate of 0.7 nm/s-0.8 nm/s;
step three: repeating the first step and the second step, and alternately plating the 3 rd to 22 th film layers;
step four: the temperature of the vacuum chamber is cooled to be lower than 50 ℃ after the plating is finished.
The further technical scheme of the invention is as follows: in the first step, before the 1 st layer of film is plated, the plated substrate of the part to be plated is cleaned and baked.
The further technical scheme of the invention is as follows: the cleaning adopts a cleaning agent.
The further technical scheme of the invention is as follows: the specific baking method comprises the following steps: to be plated withPlacing the piece in high vacuum coating equipment, vacuumizing to less than or equal to 1.0 multiplied by 10-3And Pa, and preserving the heat for 1-2 hours at 140-150 ℃.
Advantageous effects
The invention has the beneficial effects that: the invention adopts a 22-layer optimized 1.064 mu m, 7.7 mu m-10.3 mu m dual-band beam splitting film system, when the film system is incident at 45 degrees, the required reflectivity of a 1.064 mu m laser band is more than 98.00 percent, and the test value is 98.25 percent; the average value of the transmittance required by the long-wave infrared band of 7.7-10.3 microns is more than 98.50%, and the average value of the transmittance required by the test is 98.71%.
The invention strictly executes the program to set the process parameters (geometric thickness, temperature, deposition rate and vacuum degree) of each layer of coating film, and controls the geometric thickness of the film layer by combining with the film layer thickness online control system, thus realizing the preparation of the laser long-wave infrared beam splitter film of the monocrystalline germanium infrared crystal beam splitter and finally achieving the required optical characteristic technical index.
Drawings
FIG. 1 is a reflection design curve diagram of a multispectral zinc sulfide optical window provided by the present invention within a 1.064 μm waveband and 45 ° incident angle range;
FIG. 2 is a graph of the transmittance design curve of the multispectral zinc sulfide optical window provided by the present invention at a wavelength range of 7.7 μm to 10.3 μm and an incident angle range of 45 °.
Detailed Description
The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the embodiment, the film system of the laser long-wave infrared beam splitting film of the monocrystalline germanium infrared crystal spectroscope consists of 22 layers from inside to outside, and the film materials of the odd film layers are all YbF3Even number of film layers are ZnS, the geometric thickness of the layer 1 is 145.28nm, the geometric thickness of the layer 2 is 437.03nm, the geometric thickness of the layer 3 is 50.00nm, the geometric thickness of the layer 4 is 416.83nm, the geometric thickness of the layer 5 is 196.36nm, the geometric thickness of the layer 6 is 97.66nm, the geometric thickness of the layer 7 is 278.71nm, the geometric thickness of the layer 8 is 54.03nm, the geometric thickness of the layer 9 is 311.65nm, the geometric thickness of the layer 10 is 50.60nm, the geometric thickness of the layer 11 is 288.91nm, the geometric thickness of the layer 12 is 86.06nm, and the geometric thickness of the layer 13 is severalThe thickness is 223.21nm, the geometric thickness of the 14 th layer is 129.89nm, the geometric thickness of the 15 th layer is 158.52nm, the geometric thickness of the 16 th layer is 632.23nm, the geometric thickness of the 17 th layer is 171.26nm, the geometric thickness of the 18 th layer is 129.94nm, the geometric thickness of the 19 th layer is 644.37nm, the geometric thickness of the 20 th layer is 50.00nm, the geometric thickness of the 21 st layer is 682.16nm, and the geometric thickness of the 22 th layer is 91.16 nm.
The equipment used in the film system preparation process is required to be provided with a high vacuum air pumping system, two groups of resistance evaporation sources, an optical film thickness control instrument, a quartz crystal film thickness control device, an ion beam auxiliary device, a heating and baking device, a workpiece clamp with adjustable rotating speed and the like.
The film system preparation method of the single crystal germanium infrared crystal spectroscope laser long-wave infrared beam splitting film in the embodiment comprises the following steps:
1. preparation work
(1) Cleaning a vacuum chamber, a coating clamp, an evaporation source baffle, an ion source and the like;
(2) YbF is filled in the evaporation boat3、ZnS；
(3) Replacing the quartz crystal vibrating piece;
2. cleaning element
(1) The part is a monocrystalline germanium infrared crystal spectroscope;
(2) cleaning the surface of the part by using absorbent cotton dipped with alcohol ether mixed liquid;
(3) and installing a special tool and loading the parts into a vacuum chamber.
3. Film coating
Because there is certain proportion, its ratio with part rete thickness in quartz monitoring piece:
tf (correction factor) monitoring sheet thickness/part film thickness
Single-layer test ZnS and YbF on the surface of multispectral zinc sulfide infrared optical window3Thin film materials tested, the calculated Tf values are shown below:
TfZnS＝0.96；TfYbF3＝0.92
the actual plated film system structure on the quartz crystal wafer is as follows:
ZnS|0.6523L3.1922H0.2245L3.0446H0.8815L0.7134H1.2513L0.3947H1.3992L0.3696H1.2971L0.6286H10022L0.9488H0.7117L4.6180H0.7688L0.9492H2.8929L0.3652H3.0626L0.6659H | Air; (wherein H represents ZnS material, L represents YbF3Material)
Closing the vacuum chamber, starting a film coating program to start film coating, and specifically comprising the following steps:
(1) air exhausting and baking the substrate: placing the part to be plated in high vacuum plating equipment, vacuumizing to less than or equal to 1.0 multiplied by 10-3Pa, heating the substrate to 150 ℃, preserving the heat for 2 hours, and then starting an ion source to bombard the substrate for 5 min;
(2) plating a 1 st film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(3) plating a 2 nd layer film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(4) plating a 3 rd film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(5) plating a 4 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(6) plating a 5 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(7) plating a 6 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, the evaporation rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(8) plating a 7 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10-3Pa, evaporation rate of 0.9nm/s, film thickness of quartz crystal filmControlling a thickness measuring device;
(9) plating an 8 th film layer: the film material ZnS is evaporated by a resistance evaporation source, the evaporation vacuum degree is less than or equal to 1.0 multiplied by 10 < -3 > Pa, the evaporation rate is 0.8nm/s, and the film thickness is controlled by a quartz crystal film thickness measuring device;
(10) plating a 9 th film layer: membrane material YbF3Evaporating by a resistance evaporation source, wherein the evaporation vacuum degree is less than or equal to 1.0 multiplied by 10 < -3 > Pa, the evaporation rate is 0.9nm/s, and the thickness of a film layer is controlled by a quartz crystal film thickness measuring device;
(11) plating a 10 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(12) plating an 11 th film layer: membrane material YbF3Evaporating by a resistance evaporation source, wherein the evaporation vacuum degree is less than or equal to 1.0 multiplied by 10 < -3 > Pa, the evaporation rate is 0.9nm/s, and the thickness of a film layer is controlled by a quartz crystal film thickness measuring device;
(13) plating a 12 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(14) plating a 13 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(15) plating a 14 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(16) plating a 15 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(17) plating a 16 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, evaporation rateThe rate is 0.8m/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(18) plating a 17 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(19) plating an 18 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(20) plating a 19 th film layer: membrane material YbF3Evaporating by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.9nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(21) plating a 20 th film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(22) plating a 21 st film layer: membrane material YbF3Evaporating by a resistance evaporation source, wherein the evaporation vacuum degree is less than or equal to 1.0 multiplied by 10 < -3 > Pa, the evaporation rate is 0.9nm/s, and the thickness of a film layer is controlled by a quartz crystal film thickness measuring device;
(23) plating a 22 nd film layer: the film material ZnS is evaporated by a resistance evaporation source with the vacuum degree of less than or equal to 1.0 multiplied by 10- 3Pa, the evaporation rate is 0.8nm/s, and the thickness of the film layer is controlled by a quartz crystal film thickness measuring device;
(24) the temperature of the vacuum chamber is cooled to be lower than 50 ℃ after the plating is finished.
Test examples
The film systems of the examples were subjected to optical property tests, and the results of the measurements are shown in Table 1.
TABLE 1 index of optical characteristics of the plated film layer
| Operating band | 1.064μm | 7.7μm～10.3μm |
| Optical characteristics | The reflectivity is 98.25 percent | The transmittance is 98.50 percent |
As can be seen from Table 1, the reflectivity of the laser band of 1.064 μm of the film system plated in the example was 98.25% at 45 ° incidence; the average value of the transmittance test of the long-wave infrared band with the wavelength of 7.7-10.3 mu m is 98.71 percent, and the requirement of the single crystal germanium infrared crystal spectroscope beam splitting film on the optical characteristic is met.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (8)
1. A single crystal germanium infrared crystal beamsplitter, comprising: the device comprises a substrate and a beam splitting film plated on the substrate, wherein the substrate is a single crystal germanium infrared crystal, and the beam splitting film is a laser long-wave infrared beam splitting film.
2. A single crystal germanium ir crystal beamsplitter as defined in claim 1, wherein: when the beam splitting film is incident at 45 degrees, the reflectivity test value of a 1.064 mu m laser waveband is 98.25%; the average value of the transmittance test of the long-wave infrared band with the wavelength of 7.7-10.3 mu m is 98.71 percent.
3. A single crystal germanium ir crystal beamsplitter as defined in claim 1, wherein: what is needed isThe film system of the laser long-wave infrared beam splitting film comprises 22 layers from inside to outside, wherein the film materials of the odd film layers are YbF3And the film materials of the even film layers are ZnS.
4. A single crystal germanium ir crystal beamsplitter as defined in claim 3, wherein: the geometric thicknesses of the film system 22 layers are respectively as follows: layer 1 geometric thickness 145.28nm, layer 2 geometric thickness 437.03nm, layer 3 geometric thickness 50.00nm, layer 4 geometric thickness 416.83nm, layer 5 geometric thickness 196.36nm, layer 6 geometric thickness 97.66nm, layer 7 geometric thickness 278.71nm, layer 8 geometric thickness 54.03nm, layer 9 geometric thickness 311.65nm, layer 10 geometric thickness 50.60nm, layer 11 geometric thickness 288.91nm, layer 12 geometric thickness 86.06nm, layer 13 geometric thickness 223.21nm, layer 14 geometric thickness 129.89nm, layer 15 geometric thickness 158.52nm, layer 16 geometric thickness 632.23nm, layer 17 geometric thickness 171.26nm, layer 18 geometric thickness 129.94nm, layer 19 geometric thickness 644.37nm, layer 20 geometric thickness 50.00nm, layer 21 geometric thickness 682.16nm, layer 22 geometric thickness 91.16 nm.
5. A method for preparing a laser long-wave infrared beam splitting film of a single crystal germanium infrared crystal spectroscope as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
the method comprises the following steps: plating a 1 st film layer: taking YbF3The film material is evaporated by a resistance evaporation source with the vacuum degree less than or equal to 1.0 multiplied by 10-3Pa, evaporation rate of 0.8 nm/s-0.9 nm/s;
step two: plating a 2 nd layer film layer: taking ZnS film material to carry out evaporation by a resistance evaporation source, wherein the vacuum degree is less than or equal to 1.0 multiplied by 10-3Pa, evaporation rate of 0.7 nm/s-0.8 nm/s;
step three: repeating the first step and the second step, and alternately plating the 3 rd to 22 th film layers;
step four: the temperature of the vacuum chamber is cooled to be lower than 50 ℃ after the plating is finished.
6. The method for preparing a laser long-wave infrared beam splitting film of a single-crystal germanium infrared crystal spectroscope according to claim 5, wherein the method comprises the following steps: in the first step, before the 1 st layer of film is plated, the plated substrate of the part to be plated is cleaned and baked.
7. The method for preparing a laser long-wave infrared beam splitting film of a single-crystal germanium infrared crystal spectroscope according to claim 6, wherein the method comprises the following steps: the cleaning adopts a cleaning agent.
8. The method for preparing a laser long-wave infrared beam splitting film of a single-crystal germanium infrared crystal spectroscope according to claim 6, wherein the method comprises the following steps: the specific baking method comprises the following steps: placing the part to be plated in high vacuum plating equipment, vacuumizing to less than or equal to 1.0 multiplied by 10- 3And Pa, and preserving the heat for 1-2 hours at 140-150 ℃.
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| CN116240498A (en) * | 2023-03-10 | 2023-06-09 | 安徽光智科技有限公司 | Preparation method of 1064nm infrared antireflection film system of zinc selenide substrate |
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| CN116240498A (en) * | 2023-03-10 | 2023-06-09 | 安徽光智科技有限公司 | Preparation method of 1064nm infrared antireflection film system of zinc selenide substrate |
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