CN116024535A - Method and equipment for preparing radiation film, radiation film and optical device - Google Patents
Method and equipment for preparing radiation film, radiation film and optical device Download PDFInfo
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- CN116024535A CN116024535A CN202310315033.4A CN202310315033A CN116024535A CN 116024535 A CN116024535 A CN 116024535A CN 202310315033 A CN202310315033 A CN 202310315033A CN 116024535 A CN116024535 A CN 116024535A
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000005855 radiation Effects 0.000 title claims abstract description 37
- 230000003287 optical effect Effects 0.000 title claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 135
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 135
- 239000000758 substrate Substances 0.000 claims abstract description 118
- 239000011651 chromium Substances 0.000 claims abstract description 99
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 98
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 98
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- 238000001704 evaporation Methods 0.000 claims description 26
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 238000001039 wet etching Methods 0.000 claims description 15
- 229960000583 acetic acid Drugs 0.000 claims description 14
- 239000012362 glacial acetic acid Substances 0.000 claims description 14
- 229920002120 photoresistant polymer Polymers 0.000 claims description 13
- 238000004804 winding Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
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- 238000005452 bending Methods 0.000 claims description 9
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- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims description 8
- 238000002955 isolation Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000010445 mica Substances 0.000 claims description 7
- 229910052618 mica group Inorganic materials 0.000 claims description 7
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
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- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 10
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- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention provides a method and equipment for preparing a radiation film, the radiation film and an optical device, wherein the method comprises the following steps: preparing a polyimide film on the surface of a substrate; preparing a chromium adhesion layer with patterns on a polyimide film of a substrate; an aluminum black film was prepared on the chromium adhesion layer to form a radiation film. By using the scheme of the invention, the film with low density and broadband infrared absorption can be manufactured, and the manufactured film can be applied to devices such as heat detectors, heat radiators and the like to enhance photo-thermal response performance. The invention relates to the field of optical device preparation.
Description
Technical Field
The present invention relates to the field of optical device fabrication, and more particularly to a method, apparatus, radiation film, and optical device for the fabrication of radiation film.
Background
One of the currently popular heat absorbing materials is "black silicon", and black silicon research is mainly directed to the field of solar cells, if in the field of thermal imaging, the spectrum band needs to be expanded to medium and long waves, and the thickness of the nano cone needs to be increased, but this greatly increases the thermal quality of suspended pixels and reduces the sensitivity of thermal response.
Disclosure of Invention
In view of the above, an object of the embodiments of the present invention is to provide a method, an apparatus, a radiation thin film, and an optical device for manufacturing a radiation thin film, which can be used in a heat detector, a heat radiator, etc. to enhance photo-thermal response performance by using the technical scheme of the present invention to manufacture a thin film having low density and broadband infrared absorption.
In view of the above object, an aspect of an embodiment of the present invention provides a method for preparing a radiation film, including the steps of:
preparing a polyimide film on the surface of a substrate;
preparing a chromium adhesion layer with patterns on a polyimide film of a substrate;
an aluminum black film was prepared on the chromium adhesion layer to form a radiation film.
According to one embodiment of the present invention, before the polyimide film is prepared on the surface of the substrate, further comprising:
drying and cleaning a substrate, and vacuum-adsorbing the substrate on a turntable, wherein the substrate is a silicon substrate;
and preparing a polyimide film on the upper surface of the substrate.
According to one embodiment of the present invention, preparing a polyimide film on a surface of a substrate includes:
coating a polyamic acid solution on the center of the substrate;
controlling the rotation of the turntable to uniformly spread the polyamic acid solution on the whole substrate to obtain a polyamic acid film;
imidizing the polyamic acid film to obtain a polyimide film.
According to one embodiment of the present invention, coating the polyamic acid solution on the center of the substrate includes:
sucking the upper polyamide acid solution by using a clean and dry plastic dropper;
the drawn upper polyamic acid solution is coated on the central area of the substrate.
According to one embodiment of the present invention, controlling rotation of the turntable to uniformly spread the polyamic acid solution over the entire substrate to obtain a polyamic acid film includes:
the turntable is controlled to rotate at a first rotation speed for a first time so as to uniformly spread the polyamic acid solution on the substrate;
controlling the turntable to rotate at a second rotating speed for a second time to obtain a polyamic acid film with a preset thickness;
the substrate and polyamic acid film were allowed to stand at room temperature for a third time.
According to one embodiment of the present invention, imidizing the polyamic acid film to obtain a polyimide film includes:
filling nitrogen into a chamber where the polyamic acid film is positioned;
imidizing the polyamic acid film, and cooling the polyamic acid film to room temperature to obtain a polyimide film.
According to one embodiment of the present invention, preparing a patterned chromium adhesion layer on a polyimide film of a substrate includes:
preparing a chromium adhesion layer on the polyimide film;
and etching the chromium adhesion layer by adopting a wet etching method to form a preset pattern.
According to one embodiment of the present invention, preparing a chromium adhesion layer on a polyimide film includes:
cleaning impurities on the surfaces of chromium particles;
the cleaned chromium particles were evaporated using an electron beam evaporation coater to prepare a chromium adhesion layer on the polyimide film.
According to one embodiment of the present invention, etching the chromium adhesion layer to form the predetermined pattern using a wet etching method includes:
etching the chromium adhesion layer by using an etching solution comprising ceric ammonium nitrate powder, glacial acetic acid and deionized water to form a preset pattern.
According to one embodiment of the present invention, etching the chromium adhesion layer to form the predetermined pattern using a wet etching method includes:
coating photoresist with a preset pattern on the chromium adhesion layer;
the chromium adhesion layer is immersed in the etching solution at room temperature until the exposed area is completely etched.
According to one embodiment of the present invention, preparing an aluminum black film on a chromium adhesion layer to form a radiation film includes:
a first heating source and a second heating source are arranged at the bottom of the equipment;
bending a first tungsten wire into a preset shape, and connecting two ends of the first tungsten wire to positive and negative electrodes of a first heating source;
winding an aluminum wire on the first tungsten wire;
the second tungsten wire is wound into a spring-like tungsten wire coil, and both ends of the tungsten wire coil are connected to the positive and negative electrodes of the second heating source.
According to one embodiment of the present invention, bending a first tungsten wire into a predetermined shape and connecting both ends of the first tungsten wire to positive and negative electrodes of a first heating source includes:
bending the first tungsten wire into a V shape, and placing the vertex angle of the V-shaped tungsten wire downwards;
the two ends of the first tungsten wire are connected to the positive and negative electrodes of the first heating source to heat the first tungsten wire.
According to one embodiment of the present invention, winding an aluminum wire on a first tungsten wire includes:
winding aluminum wires at the vertex angles of the first tungsten wires, and enabling the wound aluminum wires to form a sphere shape.
According to one embodiment of the present invention, preparing an aluminum black film on a chromium adhesion layer to form a radiation film includes:
vacuumizing the equipment chamber, and heating the tungsten wire coil to remove oxygen and water vapor in the equipment;
isolating the aluminum wire from the film on the substrate;
introducing protective gas into the equipment;
and heating the first tungsten wire until the aluminum wire is completely melted, and removing the isolation to form an aluminum black film on the chromium adhesion layer.
According to one embodiment of the invention, isolating an aluminum wire from a film on a substrate includes:
and a mica heat insulation baffle is arranged between the aluminum wires and the film on the substrate so as to isolate the aluminum wires from the film on the substrate.
According to one embodiment of the present invention, heating the first tungsten wire until the aluminum wire is completely melted and then removing the spacers to form an aluminum black film on the chromium adhesion layer comprises:
heating the first tungsten wire until the aluminum wire is completely melted, and removing isolation;
controlling the current of the first heating source to control the evaporation rate of the aluminum wire;
and in response to the aluminum black film on the chromium adhesion layer reaching a preset thickness, disconnecting the first heating source and isolating the aluminum wires from the aluminum black film.
According to one embodiment of the present invention, further comprising:
and (3) baking the aluminum black film on the substrate at a high temperature of 100-120 ℃ for 1 hour to improve the adhesiveness of the aluminum black film.
In another aspect of embodiments of the present invention, there is also provided a radiation film manufactured using the method of manufacturing a radiation film according to any one of the above.
In another aspect of embodiments of the present invention, there is also provided an optical device comprising a radiation film as above.
In another aspect of an embodiment of the present invention, there is also provided an apparatus for preparing a radiation film, including:
a vacuum chamber;
the substrate tray is arranged at the upper part of the vacuum cavity and used for adsorbing the substrate;
the first heating source and the second heating source are arranged at the bottom of the vacuum cavity and comprise positive and negative electrodes;
the first tungsten wire is a V-shaped tungsten wire, two ends of the first tungsten wire are connected to the positive electrode and the negative electrode of the first heating source, and aluminum wires are wound at the top corners of the first tungsten wire;
the second tungsten wire is wound into a spring-shaped tungsten wire coil, and two ends of the tungsten wire coil are connected to the positive electrode and the negative electrode of the second heating source;
and the partition plate is arranged in the middle of the vacuum cavity and is configured to isolate the first tungsten wire from the substrate tray.
The invention has the following beneficial technical effects: according to the method for preparing the radiation film, provided by the embodiment of the invention, the polyimide film is prepared on the surface of the substrate; preparing a chromium adhesion layer with patterns on a polyimide film of a substrate; according to the technical scheme, the aluminum black film is prepared on the chromium adhesion layer to form the radiation film, the film with low density and broadband infrared absorption can be prepared, and the prepared film can be applied to devices such as a heat detector and a heat radiator to enhance the photo-thermal response performance.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are necessary for the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention and that other embodiments may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method of preparing a radiation film according to one embodiment of the invention;
FIG. 2 is a schematic flow chart of a method of preparing a PI film on the surface of a substrate according to one embodiment of the invention;
FIG. 3 is a schematic flow chart of a method of preparing a patterned chromium adhesion layer on a PI film of a substrate according to one embodiment of the invention;
FIG. 4 is a schematic flow chart of a method of preparing an aluminum black film on a chromium adhesion layer according to one embodiment of the invention;
fig. 5 is a schematic view of an apparatus for preparing a radiation film according to an embodiment of the present invention.
Detailed Description
In order to provide a better understanding of the present application, those skilled in the art will now make further details of the present application with reference to the drawings and detailed description. It will be apparent that the described embodiments are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
In view of the above object, a first aspect of the embodiments of the present invention proposes an embodiment of a method for producing a radiation film. Fig. 1 shows a schematic flow chart of the method.
As shown in fig. 1, the method may include the steps of:
s1 a PI (Polyimide) film is prepared on the surface of a substrate. The substrate can be a silicon substrate, the silicon substrate needs to be cleaned and dried before preparation, PAA (polyamide acid) solution with the viscosity of 300-400cps and the solid content of 12% -13% can be used for preparing the PI film, other solutions can be used according to the requirement or the viscosity and the solid content of the PAA solution can be adjusted, and the invention is not limited. The PAA solution is coated on the center of the silicon substrate and then coated on the whole silicon substrate to form a PAA film with a certain thickness, and then the PAA film is subjected to imidization treatment by using a high-temperature oven to form a PI film on the surface of the substrate.
S2, preparing a chromium adhesion layer with patterns on the PI film of the substrate. The method for preparing the chromium adhesion layer is not limited, in some embodiments, the thickness of the chromium adhesion layer is 40nm, and the chromium adhesion layer needs to be etched according to the shape of a device or a required pattern after the preparation of the chromium adhesion layer is finished, so that the chromium adhesion layer forms a desired pattern, and the chromium adhesion layer with a preset pattern is formed on the surface of the PI film after the etching is finished. The etching method can be dry etching or wet etching, and in the example of the invention, the chromium adhesion layer is etched by using wet etching, and the etching solution (etching solution) is prepared by using ceric ammonium nitrate powder, glacial acetic acid and deionized water.
S3, preparing an aluminum black film on the chromium adhesion layer to form a radiation film. The preparation of the aluminum black film can use equipment such as a resistance evaporation coating machine, a first heating source can be arranged at the bottom of the equipment, the first tungsten wire is bent into a V shape, two ends of the first tungsten wire are connected to positive and negative electrodes of the first heating source, an aluminum wire is wound on the V-shaped vertex angle of the first tungsten wire, the aluminum wire is wound into a sphere, the tungsten wire is heated by a first power supply so as to melt and evaporate the aluminum wire, evaporated metal particles are attached to a chromium attachment layer to form the aluminum black film, the first tungsten wire is bent into the V shape, the resistance of the vertex angle can be improved, and the aluminum wire is easier to melt and evaporate. The aluminum black film is a sparse porous low-density metal black film, the porous structure is similar to a blackbody cavity, incident light can be absorbed, the random size of the holes can greatly expand the width of an absorption wave band, and various low-melting-point metals such as gold, silver, aluminum and the like can be used for preparing the black film.
By using the technical scheme of the invention, the film with low density and broadband infrared absorption can be prepared, and the prepared film can be applied to devices such as a heat detector, a heat radiator and the like to enhance the photo-thermal response performance.
In a preferred embodiment of the present invention, before the PI film is prepared on the surface of the substrate, further comprising:
drying and cleaning a substrate, and vacuum-adsorbing the substrate on a turntable, wherein the substrate is a silicon substrate;
and preparing a PI film on the upper surface of the substrate. In order to avoid adverse effects of impurities on the substrate on the PI film, the substrate needs to be cleaned before the PI film is prepared, dirt on the surface of the substrate is removed, the cleanliness of the substrate is improved, the substrate needs to be dried after the substrate is cleaned, and the influence of residual moisture on the PI film is avoided. After the substrate is dried and cleaned, the substrate is placed on a rotary table and is adsorbed on the rotary table, the rotary table can rotate at different speeds at uniform speed, and the rotary table rotates to drive the substrate on the rotary table to rotate so as to prepare the PI film. The substrate can be a silicon substrate, or other materials can be selected as required as the substrate, and the invention is not limited.
In a preferred embodiment of the present invention, as shown in fig. 2, preparing a PI film on the surface of a substrate includes:
s11, coating PAA solution on the center of a substrate;
s12, controlling the turntable to rotate so as to uniformly spread the PAA solution on the whole substrate, thereby obtaining a PAA film;
s13, imidizing the PAA film to obtain a PI film. In the present example, the PI film is prepared by using a spin coating method, which is a typical flexible film preparation process, and the film thickness is related to the rotation speed, the solution viscosity, the curing temperature, etc., the present invention uses the PAA solution with the viscosity of 300-400cps and the solid content of 12% -13% as an example, and other solutions can be used or the viscosity and the solid content of the PAA solution can be adjusted as required, and the present invention is not limited. The PAA solution is coated on the center of the substrate, then the turntable is controlled to rotate at a certain speed, the PAA solution can be uniformly spread on the whole substrate, then the turntable is controlled to rotate in an accelerating way for a certain time, a PAA film with a certain thickness can be obtained, the thickness of the PAA film can be set according to the requirement, meanwhile, the rotating speed and time of the turntable are controlled according to the set thickness, and finally the PAA film is subjected to imidization treatment to obtain the PI film.
In a preferred embodiment of the invention, applying the PAA solution to the center of the substrate comprises:
sucking the upper PAA solution by using a clean and dry plastic dropper;
the aspirated upper layer PAA solution is coated on the central area of the substrate. Firstly, vacuum-adsorbing a dried and cleaned silicon substrate on a spin stand (turntable) tray, then sucking a proper amount of upper PAA solution by using a clean and dry plastic dropper, coating the upper PAA solution on a region about 2/3 of the center of the substrate, avoiding air bubbles in the process of coating the PAA solution, and avoiding the PAA solution from contacting with water in use. The PAA solution can be uniformly spread over the entire substrate as the turntable rotates.
In a preferred embodiment of the present invention, controlling the rotation of the turntable to uniformly spread the PAA solution over the entire substrate to obtain the PAA film comprises:
controlling the rotary table to rotate at a first rotation speed for a first time so as to uniformly spread the PAA solution on the substrate;
controlling the turntable to rotate at a second rotating speed for a second time to obtain a PAA film with a preset thickness;
the substrate and PAA film were allowed to stand at room temperature for a third time. In the embodiment of the invention, the first rotation speed is 800rpm, the first time (spin coating time) is 60s, after the PAA solution is coated on the substrate, the turntable is controlled to rotate at the first rotation speed for 60s so that the PAA solution uniformly spreads over the whole substrate, the second rotation speed is 4000rpm, the second time (spin coating time) is 3min, after the turntable rotates at the first rotation speed for 60s, the speed of the turntable is adjusted to the second rotation speed, the turntable rotates at the second rotation speed for 3min, the purpose is to obtain the PAA film with a specific thickness, the thickness of the PAA film can be set according to the requirement, meanwhile, the rotation speed and the spin coating time of the turntable are controlled according to the set thickness, the spin coating thickness is mainly related to the high rotation speed, and the higher the rotation speed is, and the thinner the film thickness is. After spin coating, the PAA film was left to stand at room temperature for 1h to evaporate naturally the solvent NMP (N-methyl-2-pyrrolidone, N-methylpyrrolidone).
In a preferred embodiment of the present invention, imidizing the PAA film to obtain a PI film comprises:
filling nitrogen into a chamber where the PAA film is positioned;
imidizing the PAA film, and cooling the PAA film to room temperature to obtain the PI film. The PAA film is subjected to imidization treatment by using a high-temperature oven, the set temperature is respectively 1h at 200, 250 and 300 ℃, the temperature is raised stepwise, the protective gas is nitrogen, the PAA film is naturally cooled to room temperature to obtain the PI film, the thickness of the PI film prepared under the above material parameters and process parameters is about 500nm through the step meter test, and the parameter adjustment can be carried out according to specific conditions in practical application.
In a preferred embodiment of the present invention, as shown in fig. 3, preparing a chromium adhesion layer having a pattern on a PI film of a substrate includes:
s21, preparing a chromium adhesion layer on the PI film;
and S22, etching the chromium adhesion layer by adopting a wet etching method to form a preset pattern. Because the adhesion property of the aluminum black film on the PI film is poor, the invention uses the electron beam evaporation coating machine to prepare the chromium adhesion layer on the PI substrate in advance, the invention does not limit the preparation method of the chromium adhesion layer, in one embodiment of the invention, the thickness of the chromium adhesion layer is 40nm, the purity of chromium particles is 99.95%, the control parameter of evaporation is air pressure of 5 x 10 < -4 > Pa, the evaporation rate is 0.1A/s, the substrate temperature is 110 ℃, and the film thickness is controlled by a crystal oscillator wafer. The etching method may be dry etching or wet etching, in the example of the present invention, wet etching is used to etch the chromium adhesion layer, the etching solution (etching solution) is prepared by using ammonium cerium nitrate powder, glacial acetic acid and deionized water, in one embodiment of the present invention, 25g ammonium cerium nitrate powder, 20mL 36% glacial acetic acid and 100mL deionized water may be used to prepare the etching solution, and after the preparation, the transparent golden yellow solution is obtained. The Ce element in the ammonium cerium nitrate is +4, has enough oxidability, can perform oxidation-reduction reaction with metal chromium, and the glacial acetic acid is mainly used for providing an acidic environment to enhance the oxidability and does not participate in chemical reaction.
In a preferred embodiment of the present invention, preparing the chromium adhesion layer on the PI film comprises:
cleaning impurities on the surfaces of chromium particles;
the cleaned chromium particles were evaporated using an electron beam evaporation coater to prepare a chromium adhesion layer on the PI film.
In a preferred embodiment of the present invention, etching the chromium adhesion layer to form the predetermined pattern using a wet etching method includes:
etching the chromium adhesion layer by using an etching solution comprising ceric ammonium nitrate powder, glacial acetic acid and deionized water to form a preset pattern. The aluminum black film has a sparse and porous structure, is difficult to be compatible with subsequent photoetching, etching and other patterning processes, and takes the obvious difference of the adhesion of the aluminum black film on the surface of the chromium adhesion layer and the PI film into consideration, so that the aluminum black is indirectly patterned by patterning the chromium adhesion layer. After the preparation of the chromium layer, the chromium adhesion layer needs to be etched according to the shape of the device so that the chromium adhesion layer forms a desired pattern. The etching method may be dry etching or wet etching, in the example of the present invention, wet etching is used to etch the chromium adhesion layer, the etching solution (etching solution) is prepared by using ammonium cerium nitrate powder, glacial acetic acid and deionized water, in one embodiment of the present invention, 25g ammonium cerium nitrate powder, 20mL 36% glacial acetic acid and 100mL deionized water may be used to prepare the etching solution, and after the preparation, the transparent golden yellow solution is obtained. The Ce element in the ammonium cerium nitrate is +4, has enough oxidability, can perform oxidation-reduction reaction with metal chromium, and the glacial acetic acid is mainly used for providing an acidic environment to enhance the oxidability and does not participate in chemical reaction.
In a preferred embodiment of the present invention, etching the chromium adhesion layer to form the predetermined pattern using a wet etching method includes:
coating photoresist with a preset pattern on the chromium adhesion layer;
the chromium adhesion layer is immersed in the etching solution at room temperature until the exposed area is completely etched. The photoresist can be used as a mask to coat the photoresist on the chromium layer, the photoresist needs to be coated into a preset pattern, the preset pattern is designed according to the shape or the requirement of a device, the shape of the etched chromium adhesion layer on the PI film is the same as the shape of the photoresist coating, and the chromium layer needs to be immersed into corrosive liquid at room temperature until the exposed area is completely etched after the photoresist coating is completed. In one embodiment of the invention, 25g of ammonium cerium nitrate powder, 20mL of 36% strength glacial acetic acid, and 100mL of deionized water may be used to formulate the etching solution as a clear solution of golden yellow color. The Ce element in the ammonium cerium nitrate is +4, has enough oxidability, can perform oxidation-reduction reaction with metal chromium, and the glacial acetic acid is mainly used for providing an acidic environment to enhance the oxidability and does not participate in chemical reaction. After etching is completed, the photoresist is required to be stripped, and a chromium adhesion layer with a preset pattern is formed on the PI film after the photoresist is stripped.
In a preferred embodiment of the present invention, preparing an aluminum black film on the chromium adhesion layer to form a radiation film includes:
a first heating source and a second heating source are arranged at the bottom of the equipment;
bending a first tungsten wire into a preset shape, and connecting two ends of the first tungsten wire to positive and negative electrodes of a first heating source;
winding an aluminum wire on the first tungsten wire;
the two ends of the tungsten wire coil are connected to the positive and negative electrodes of the second heating source. The equipment can use ZHD-300 resistance evaporation coating machine, and can also use other types of equipment with similar functions to manufacture the aluminum black film. Referring to fig. 5, two heating sources are required to be arranged at the bottom of the device, a first heating source is used for evaporating aluminum black, a second heating source is used for removing oxygen and water vapor in the device, two tungsten wires are required to be arranged at the bottom of the device, the first tungsten wires are required to be bent into a V shape, the top angles of the V-shaped tungsten wires are downwards arranged, aluminum wires are wound on the top angles of the first tungsten wires, the aluminum wires are wound into balls on the top angles, two ends of the first tungsten wires are connected to the positive electrode and the negative electrode of the first heating source, and the first heating source heats the first tungsten wires after the positive electrode and the negative electrode of the first heating source are electrified, so that the aluminum wires are melted and the aluminum black is evaporated. The second tungsten wire is required to be wound into a spring-shaped tungsten wire coil, the second tungsten wire is also arranged at the bottom of the device, two ends of the second tungsten wire are connected to the positive electrode and the negative electrode of the second heating source, the positive electrode and the negative electrode of the second heating source are electrified to heat the second tungsten wire, oxygen and water vapor in the device can be removed by the heated second tungsten wire, the area of the tungsten wire contacting air can be increased by winding the second tungsten wire into the tungsten wire coil, and the oxygen and the water vapor in the air can be removed more easily.
In a preferred embodiment of the present invention, bending the first tungsten wire into a predetermined shape and connecting both ends of the first tungsten wire to the positive and negative electrodes of the first heating source includes:
bending the first tungsten wire into a V shape, and placing the vertex angle of the V-shaped tungsten wire downwards;
the two ends of the first tungsten wire are connected to the positive and negative electrodes of the first heating source to heat the first tungsten wire. The first tungsten wire is required to be bent into a V shape, the vertex angle of the V-shaped tungsten wire is arranged downwards, the aluminum wire is wound on the vertex angle of the first tungsten wire, the aluminum wire is wound on the vertex angle to form a sphere, two ends of the first tungsten wire are connected to the positive electrode and the negative electrode of the first heating source, the first tungsten wire is heated after the positive electrode and the negative electrode of the first heating source are electrified, so that the aluminum wire is melted and evaporated, and the evaporation rate of the aluminum black is controlled by controlling the current of the first heating source.
In a preferred embodiment of the present invention, winding an aluminum wire on a first tungsten wire comprises:
winding aluminum wires at the vertex angles of the first tungsten wires, and enabling the wound aluminum wires to form a sphere shape.
In a preferred embodiment of the present invention, connecting both ends of the tungsten wire coil to the positive and negative electrodes of the second heating source comprises:
and winding the second tungsten wire into a spring-shaped coil, and connecting two ends of the coil wound by the tungsten wire to positive and negative electrodes of a second heating source so as to heat the second tungsten wire. The second tungsten wire is required to be wound into a spring-shaped coil, the second tungsten wire is also arranged at the bottom of the device, two ends of the second tungsten wire are connected to the positive electrode and the negative electrode of the second heating source, the positive electrode and the negative electrode of the second heating source are electrified to heat the second tungsten wire, and the heated second tungsten wire can remove oxygen and water vapor in the device.
In a preferred embodiment of the present invention, as shown in fig. 4, preparing an aluminum black film on a chromium adhesion layer to form a radiation film includes:
s31, vacuumizing the equipment chamber, and heating the tungsten wire coil to remove oxygen and water vapor in the equipment;
s32, isolating the aluminum wires from the film on the substrate;
s33, introducing protective gas into the equipment;
s34, heating the first tungsten wire until the aluminum wire is completely melted, and removing the isolation to form an aluminum black film on the chromium adhesion layer. When preparing the aluminum black film, the cavity is pumped out first10 into 10 -4 After Pa, the second heating source is electrified to heat the tungsten wire coil, residual oxygen and water vapor in the cavity can be removed when the tungsten wire coil is in a yellowing state, and the first heating source is electrified in the vacuum environment, so that the aluminum wire ball is melted by high current, and the aluminum wire needs to be isolated from a film on the substrate before the aluminum wire ball is melted, so that the damage of a sample caused by metal splashing is avoided. High-purity He gas is introduced and the stable pressure is 900Pa, and other protective gases such as argon can be used as the protective gas. The evaporation rate of the aluminum black can be controlled by controlling the first heating source current, in one embodiment of the invention, the evaporation rate of the aluminum black is about 15nm/s, the isolation between the aluminum filaments and the film on the substrate is removed when the aluminum filament ball is completely melted, and the evaporation time is controlled according to the thickness of the aluminum black film prepared as required and the evaporation rate of the aluminum black, in the example of the invention, the aluminum black film with the thickness of about 2 microns is prepared. The aluminum black can be coated on the PI film and the chromium adhesion layer in the evaporation process, but the adhesion property of the aluminum black film on the PI film is poor, so that the aluminum black film can be separated from the PI film, the adhesion property of the aluminum black film on the chromium adhesion layer is good, and the aluminum black film can be coated on the chromium adhesion layer.
In a preferred embodiment of the present invention, isolating the aluminum filaments from the film on the substrate comprises:
and a mica heat insulation baffle is arranged between the aluminum wires and the film on the substrate so as to isolate the aluminum wires from the film on the substrate. The middle part that can set up the division board at equipment, the division board can use mica thermal-insulated baffle, also can use other baffles that have the same effect, keeps apart mica thermal-insulated baffle between the film of aluminium silk and basement before aluminium silk ball melts to avoid the metal to splash to cause the destruction of sample, when aluminium silk ball accomplishes melting, get rid of the mica thermal-insulated baffle between the film on aluminium silk and the basement.
In a preferred embodiment of the present invention, heating the first tungsten wire until the aluminum wire is completely melted and then removing the spacers to form an aluminum black film on the chromium adhesion layer comprises:
heating the first tungsten wire until the aluminum wire is completely melted, and removing isolation;
controlling the current of the first heating source to control the evaporation rate of the aluminum wire;
and in response to the aluminum black film on the chromium adhesion layer reaching a preset thickness, disconnecting the first heating source and isolating the aluminum wires from the aluminum black film. By controlling the first heating source current and thus the evaporation rate of the aluminum black, in one embodiment of the invention, the evaporation rate of the aluminum black is about 15nm/s, when the aluminum wire ball is melted, the isolation between the aluminum wire and the film on the substrate is removed, the evaporation time is controlled according to the thickness of the aluminum black film prepared as required and the evaporation rate of the aluminum black, in the example of the invention, the aluminum black film with the thickness of about 2 microns is prepared, after the aluminum black film reaches the required thickness, namely 2 microns, the power of the first heating source is cut off, the continuous evaporation of the aluminum black is stopped, and meanwhile, the aluminum wire and the aluminum black film need to be isolated again.
In a preferred embodiment of the present invention, further comprising:
and (3) baking the aluminum black film on the substrate at a high temperature of 100-120 ℃ for 1 hour to improve the adhesiveness of the aluminum black film.
Examples
And 1, vacuum-adsorbing a dried and cleaned silicon substrate on a spin stand tray, sucking a proper amount of upper PAA solution by using a clean and dried plastic dropper, wherein the viscosity of the PAA solution is 300-400cps, the solid content is 12% -13%, and coating the sucked PAA solution on a region about 2/3 of the center of the substrate.
And 3, carrying out imidization treatment on the PAA film by using a high-temperature oven, setting the temperature at 200, 250 and 300 ℃ for 1h respectively, heating stepwise, using nitrogen as protective gas, and finally naturally cooling to room temperature to obtain the PI film.
And 4, preparing a chromium adhesion layer with the thickness of 40nm on the PI film, wherein the purity of chromium particles is 99.95 percent during preparation, the set air pressure is 5 multiplied by 10 < -4 > Pa, the evaporation rate is 0.1A/s, and the substrate temperature is 110 ℃.
And 5, coating the photoresist on the chromium adhesion layer in a preset pattern by using the photoresist as a mask, immersing the chromium adhesion layer in etching solution at room temperature until the exposed area is completely etched, and stripping the photoresist after etching, wherein the etching solution is prepared from 25g of ammonium cerium nitrate powder, 20mL of 36% glacial acetic acid and 100mL of deionized water, and the prepared solution is golden yellow transparent solution, wherein Ce element in the ammonium cerium nitrate is +4, has enough oxidizing property, can generate oxidation-reduction reaction with metal Cr, and the glacial acetic acid is mainly used for providing acidic environment to enhance oxidizing property and does not participate in chemical reaction.
And 6, preparing a metal aluminum black film by using a ZHD-300 type resistance evaporation coating machine, designing two heating sources at the bottom of the coating machine, wherein the first heating source is used for evaporating aluminum black, and the second heating source is used for removing oxygen and water vapor in the cavity. The method comprises the steps of placing a high-melting-point first tungsten wire bent into a V-shaped angle of 45 degrees at the bottom of a film plating machine, winding an aluminum wire with the diameter of 0.5mm and the length of 6cm at the vertex angle of the V into a sphere to be heated and melted, fixing two ends of the first tungsten wire on a positive electrode and a negative electrode of a first heating source, controlling the evaporation rate through current, winding a second tungsten wire into a spring-shaped coil, and connecting two ends of the tungsten wire coil with the positive electrode and the negative electrode of the second heating source to remove residual oxygen.
And 7, after the chamber is pumped into 10 < -4 > Pa, heating the tungsten wire coil to a yellowing state so as to remove residual oxygen and water vapor, in the vacuum environment, melting aluminum wire balls through high current of a first heating source, isolating the aluminum wires from a film of a substrate by using a mica heat insulation baffle, avoiding damage of a sample caused by metal splashing, introducing high-purity He gas, stabilizing the air pressure at 900Pa, opening the baffle for timing evaporation after controlling the evaporation rate to be about 15nm/s by controlling the current of the first heating source, and preparing an aluminum black film with the thickness of about 2 microns, and after the evaporation is finished, baking the aluminum black film at a high temperature of 100-120 ℃ so as to improve the adhesiveness of aluminum black.
By using the technical scheme of the invention, the film with low density and broadband infrared absorption can be prepared, and the prepared film can be applied to devices such as a heat detector, a heat radiator and the like to enhance the photo-thermal response performance.
In view of the above object, a second aspect of the embodiments of the present invention provides a radiation film manufactured by the method of manufacturing a radiation film according to any one of the above.
In view of the above object, a third aspect of an embodiment of the present invention proposes an optical device comprising a radiation film as above.
In view of the above object, a fourth aspect of the embodiments of the present invention provides an apparatus for preparing a radiation film, as shown in fig. 5, comprising:
a vacuum chamber 1;
a substrate tray 2, the substrate tray 2 being disposed at an upper portion of the vacuum chamber 1 for adsorbing a substrate 3;
a first heating source 5 and a second heating source 6, the first heating source 5 and the second heating source 6 being disposed at the bottom of the vacuum chamber 1 and each including positive and negative electrodes;
the first tungsten wire 7 is a V-shaped tungsten wire, two ends of the first tungsten wire 7 are connected to the positive electrode and the negative electrode of the first heating source 5, and aluminum wires 9 are wound at the top corners of the first tungsten wire 7;
a second tungsten wire 8, the second tungsten wire 8 being wound into a spring-like tungsten wire coil, both ends of the tungsten wire coil being connected to the positive and negative electrodes of the second heating source 6;
and a partition board 4, wherein the partition board 4 is arranged in the middle of the vacuum cavity 1 and is configured to isolate the first tungsten wire 7 from the substrate tray 3. The equipment is mainly used for preparing the aluminum black film, and after the PI film and the chromium adhesion layer are prepared on the substrate, the equipment can be used for preparing the aluminum black film on the chromium adhesion layer.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the disclosure as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
It should be understood that as used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly supports the exception. It should also be understood that "and/or" as used herein is meant to include any and all possible combinations of one or more of the associated listed items.
Those of ordinary skill in the art will appreciate that: the above discussion of any embodiment is merely exemplary and is not intended to imply that the scope of the disclosure of embodiments of the invention, including the claims, is limited to such examples; combinations of features of the above embodiments or in different embodiments are also possible within the idea of an embodiment of the invention, and many other variations of the different aspects of the embodiments of the invention as described above exist, which are not provided in detail for the sake of brevity. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the embodiments should be included in the protection scope of the embodiments of the present invention.
Claims (20)
1. A method for preparing a radiation film, comprising the steps of:
preparing a polyimide film on the surface of a substrate;
preparing a chromium adhesion layer with patterns on a polyimide film of a substrate;
an aluminum black film was prepared on the chromium adhesion layer to form a radiation film.
2. The method of claim 1, further comprising, prior to preparing the polyimide film on the surface of the substrate:
drying and cleaning a substrate, and vacuum-adsorbing the substrate on a turntable, wherein the substrate is a silicon substrate;
and preparing a polyimide film on the upper surface of the substrate.
3. The method of claim 1, wherein preparing a polyimide film on a surface of a substrate comprises:
coating a polyamic acid solution on the center of the substrate;
controlling the rotation of the turntable to uniformly spread the polyamic acid solution on the whole substrate to obtain a polyamic acid film;
imidizing the polyamic acid film to obtain a polyimide film.
4. The method of claim 3, wherein applying the polyamic acid solution to the center of the substrate comprises:
sucking the upper polyamide acid solution by using a clean and dry plastic dropper;
the drawn upper polyamic acid solution is coated on the central area of the substrate.
5. The method of claim 3, wherein controlling the rotation of the turntable to uniformly spread the polyamic acid solution over the entire substrate to obtain the polyamic acid film comprises:
the turntable is controlled to rotate at a first rotation speed for a first time so as to uniformly spread the polyamic acid solution on the substrate;
controlling the turntable to rotate at a second rotating speed for a second time to obtain a polyamic acid film with a preset thickness;
the substrate and polyamic acid film were allowed to stand at room temperature for a third time.
6. The method of claim 3, wherein imidizing the polyamic acid film to obtain a polyimide film comprises:
filling nitrogen into a chamber where the polyamic acid film is positioned;
imidizing the polyamic acid film, and cooling the polyamic acid film to room temperature to obtain a polyimide film.
7. The method of claim 1, wherein preparing a patterned chromium adhesion layer on a polyimide film of a substrate comprises:
preparing a chromium adhesion layer on the polyimide film;
and etching the chromium adhesion layer by adopting a wet etching method to form a preset pattern.
8. The method of claim 7, wherein preparing a chromium adhesion layer on the polyimide film comprises:
cleaning impurities on the surfaces of chromium particles;
the cleaned chromium particles were evaporated using an electron beam evaporation coater to prepare a chromium adhesion layer on the polyimide film.
9. The method of claim 7, wherein etching the chromium adhesion layer to form the predetermined pattern using a wet etching method comprises:
etching the chromium adhesion layer by using an etching solution comprising ceric ammonium nitrate powder, glacial acetic acid and deionized water to form a preset pattern.
10. The method of claim 7, wherein etching the chromium adhesion layer to form the predetermined pattern using a wet etching method comprises:
coating photoresist with a preset pattern on the chromium adhesion layer;
the chromium adhesion layer is immersed in the etching solution at room temperature until the exposed area is completely etched.
11. The method of claim 1, wherein preparing an aluminum black film on the chromium adhesion layer to form the radiant film comprises:
a first heating source and a second heating source are arranged at the bottom of the equipment;
bending a first tungsten wire into a preset shape, and connecting two ends of the first tungsten wire to positive and negative electrodes of a first heating source;
winding an aluminum wire on the first tungsten wire;
and winding a second tungsten wire into a spring-shaped tungsten wire coil, and connecting two ends of the tungsten wire coil to the positive electrode and the negative electrode of the second heating source.
12. The method of claim 11, wherein bending the first tungsten wire into a predetermined shape and connecting both ends of the first tungsten wire to the positive and negative electrodes of the first heating source comprises:
bending the first tungsten wire into a V shape, and placing the vertex angle of the V-shaped tungsten wire downwards;
the two ends of the first tungsten wire are connected to the positive and negative electrodes of the first heating source to heat the first tungsten wire.
13. The method of claim 12, wherein wrapping aluminum wire around the first tungsten wire comprises:
winding aluminum wires at the vertex angles of the first tungsten wires, and enabling the wound aluminum wires to form a sphere shape.
14. The method of claim 11, wherein preparing an aluminum black film on the chromium adhesion layer to form the radiant film comprises:
vacuumizing the equipment chamber, and heating the tungsten wire coil to remove oxygen and water vapor in the equipment;
isolating the aluminum wire from the film on the substrate;
introducing protective gas into the equipment;
and heating the first tungsten wire until the aluminum wire is completely melted, and removing the isolation to form an aluminum black film on the chromium adhesion layer.
15. The method of claim 14, wherein isolating the aluminum filaments from the film on the substrate comprises:
and a mica heat insulation baffle is arranged between the aluminum wires and the film on the substrate so as to isolate the aluminum wires from the film on the substrate.
16. The method of claim 14, wherein heating the first tungsten filament to completely melt the aluminum filament and then removing the spacers to form an aluminum black film on the chromium adhesion layer comprises:
heating the first tungsten wire until the aluminum wire is completely melted, and removing isolation;
controlling the current of the first heating source to control the evaporation rate of the aluminum wire;
and in response to the aluminum black film on the chromium adhesion layer reaching a preset thickness, disconnecting the first heating source and isolating the aluminum wires from the aluminum black film.
17. The method as recited in claim 16, further comprising:
and (3) baking the aluminum black film on the substrate at a high temperature of 100-120 ℃ for 1 hour to improve the adhesiveness of the aluminum black film.
18. A radiation film produced by the method of producing a radiation film according to any one of claims 1 to 17.
19. An optical device comprising the radiation film of claim 18.
20. An apparatus for producing a radiation film, comprising:
a vacuum chamber;
the substrate tray is arranged at the upper part of the vacuum cavity and used for adsorbing the substrate;
the first heating source and the second heating source are arranged at the bottom of the vacuum cavity and comprise positive and negative electrodes;
the first tungsten wire is a V-shaped tungsten wire, two ends of the first tungsten wire are connected to the positive electrode and the negative electrode of the first heating source, and aluminum wires are wound at the top corners of the first tungsten wire;
the second tungsten wire is wound into a spring-shaped tungsten wire coil, and two ends of the tungsten wire coil are connected to the positive electrode and the negative electrode of the second heating source;
and the partition plate is arranged in the middle of the vacuum cavity and is configured to isolate the first tungsten wire from the substrate tray.
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