CN109932064B - Infrared focal plane array detector with DLC protective film and preparation method thereof - Google Patents
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Abstract
The invention provides a preparation method of an infrared focal plane array detector with a DLC protective film, which comprises the following steps: A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution; B) the cleaned infrared cokeIntroducing argon into a window of the planar array detector under a vacuum condition, and performing radio frequency plasma cleaning; C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film; the radio frequency power of the step C) is 100-2500W, and the vacuum degree of the step C) is 3 multiplied by 10‑3～3×10‑5Pa. The invention also provides an infrared focal plane array detector with the DLC protective film.
Description
Technical Field
The invention belongs to the technical field of infrared focal plane arrays, and particularly relates to an infrared focal plane array detector with a DLC (diamond-like carbon) protective film and a preparation method thereof.
Background
Over the twenty-first century, the development of infrared thermal photography has been over thirty years, and has been developed from the beginning of mechanical scanning mechanisms to the present full-solid miniaturized full-electronic scanning staring photography, and especially the development of non-refrigeration technology has expanded the infrared thermal photography from the long-term major military purpose to a wide civilian field such as industrial detection and temperature control, law enforcement and drug enforcement, safety precaution, medical hygiene, remote sensing, equipment advanced fault diagnosis and maintenance, marine rescue, astronomical exploration, vehicles, flying chess and ship drivers as well as enhanced observers.
The development speed of infrared thermal imaging technology mainly depends on the progress of infrared detector technology, and at present, an infrared focal plane array detector is formed by selecting a high-refractive-index material (such as germanium) as a base material on a chip using a vanadium oxide thin film as a thermosensitive material, and plating an anti-reflection film (such as ZnSe, ZnS and the like) on the surface of the germanium to increase the transmittance of infrared radiation. However, although the commonly used infrared antireflection film (such as ZnSe, ZnS, etc.) has excellent antireflection performance, the mechanical strength of the film itself is low, and scratch, abrasion or corrosion is easily formed in the production (especially in the assembly and debugging stages) and use processes (the infrared focal plane array detector is mostly used in extreme environments) of the vacuum window sealing window of the detector, which may cause the window antireflection film to be damaged to reduce the infrared radiation transmittance, further cause the performance of the detector to be reduced or the picture quality to be poor, and lead the detector component to be out of work, increase the production cost and reduce the service life of the product.
Disclosure of Invention
The invention aims to provide an infrared focal plane array detector with a DLC protective film and a preparation method thereof.
The invention provides a preparation method of an infrared focal plane array detector with a DLC protective film, which comprises the following steps:
A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution;
B) introducing argon into the cleaned window of the infrared focal plane array detector under a vacuum condition, and performing radio frequency plasma cleaning;
C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film;
the radio frequency power of the step C) is 100-2500W, and the vacuum degree of the step C) is 3 multiplied by 10-3～3×10- 5Pa。
Preferably, the window of the infrared focal plane array detector comprises a ZnSe layer, a ZnS layer, a Ge layer, a ZnS layer and a ZnSe layer which are sequentially contacted;
the ZnSe layer is in contact with the DLC protective film.
Preferably, the vacuum degree in the step B) is 0.0013-0.13 Pa;
the flow of argon in the step B) is 30-90 sccm;
the radio frequency power in the step B) is 300-700W.
Preferably, the carbon source gas is methane;
the flow rate of the carbon source gas is 5-100 sccm.
Preferably, the deposition temperature in the step C) is 20-200 ℃;
the deposition time in the step C) is 0.1-10 min.
Preferably, argon is used as a carrier gas in the deposition process of the step C);
the flow rate of the argon is 100-200 sccm.
Preferably, the working solution is one or more of acetone, isopropanol and N-methylpyrrolidone.
The invention provides an infrared focal plane array detector with a DLC protective film, which comprises an infrared focal plane array detector and the DLC protective film deposited on the surface of a detector window;
the infrared focal plane array detector with the DLC protective film is prepared by the preparation method of any one of claims 1 to 7.
Preferably, the working waveband of the infrared focal plane array detector with the DLC protective film is 3-5 μm or 8-14 μm.
Preferably, the DLC protective film has a refractive index of 1.8 to 3.1.
The invention provides a preparation method of an infrared focal plane array detector with a DLC protective film, which comprises the following steps: A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution; B) introducing argon into the cleaned window of the infrared focal plane array detector under a vacuum condition, and performing radio frequency plasma cleaning; C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film; the radio frequency power of the step C) is 100-2500W, and the vacuum degree of the step C) is 3 multiplied by 10-3～3×10-5Pa. The invention adopts a radio frequency Plasma Enhanced Chemical Vapor Deposition (PECVD) method to deposit the DLC film on the surface of the window of the detector, and simultaneously controls the deposition condition to ensure that the DLC film is depositedThe coating has the advantages of more uniform deposition, good film forming property, high scratch resistance, high friction resistance and high corrosion resistance while ensuring high transmittance and low infrared absorption rate. In addition, the DLC film has high deposition speed, high single-furnace yield and less damage to the substrate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of a window structure of an infrared focal plane array detector with a DLC protective film according to the present invention.
Detailed Description
The invention provides a preparation method of an infrared focal plane array detector with a DLC protective film, which comprises the following steps:
A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution;
B) introducing argon into the cleaned window of the infrared focal plane array detector under a vacuum condition, and performing radio frequency plasma cleaning;
C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film;
the radio frequency power of the step C) is 100-2500W, and the vacuum degree of the step C) is 3 multiplied by 10-3～3×10- 5Pa。
The infrared focal plane array detector absorbs infrared waves to form images, an independent infrared optical lens is additionally arranged in a terminal use scene of the detector, the detector does not directly contact the environment such as the external atmosphere, the detector is assembled into a machine core, then the machine core is assembled into a whole machine by adding the infrared lens and the like, and in the long process, the infrared optical lens or other parts do not exist to protect a window of the detector, so that the DLC film is deposited on the surface of the window to protect the detector, can protect the detector from being manufactured into the machine core, and can not be scratched and worn in the whole processing process of the whole machine and the use of subsequent products, and meanwhile, the infrared transmittance can not be reduced.
The detector window takes germanium (Ge) as a base material, and an antireflection film is plated on the surface of the Ge, and the detector window has a specific structure shown in figure 1 and comprises a ZnSe layer, a ZnS layer, a Ge layer, a ZnS layer and a ZnSe layer which are sequentially contacted; the ZnSe layer is in contact with the DLC protective film.
The invention preferably adopts a radio frequency plasma enhanced chemical vapor deposition method to deposit the DLC protective film on the surface of the infrared detector window which takes Ge as a base material and is plated with a ZnSe antireflection film. The invention preferably cleans the vacuum chamber to remove dust, and prevents the dust from polluting the substrate during vacuum pumping.
Then, the invention cleans the window substrate, and avoids the reduction of the film-substrate binding force caused by foreign matters, thereby the light-emitting rate and the refractive index of the film are influenced. Preferably, the window substrate is cleaned by acetone under ultrasound for 5-30 min to remove surface oil stains, then cleaned by working solution under ultrasound for 5-20 min, repeatedly washed by deionized water for 5-20 min to remove surface impurities, and finally dried in a drying machine.
And putting the cleaned infrared focal plane array detector window into a vacuum chamber, vacuumizing, and preparing for performing radio frequency plasma enhanced chemical vapor Deposition (DLC) film.
The invention preferably sets a vacuum degree, argon is introduced after the vacuum degree reaches a set value, the radio frequency power is adjusted, and argon ion cleaning is carried out on the surface of the window.
In the invention, the vacuum degree of the step is preferably 0.13-0.0013 Pa, more preferably 0.1-0.005 Pa, and most preferably 0.01-0.005 Pa; the flow rate of the argon gas is preferably 30-90 sccm, more preferably 40-80 sccm, and most preferably 50-70 sccm; the radio frequency power is preferably 300-700W, more preferably 300-600W, and most preferably 300W.
After the sub-ion cleaning is finished, carbon source gas is introduced, and a DLC protective film is deposited on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method, so that the infrared focal plane array detector with the DLC protective film is obtained.
The Diamond film is also called DLC film, which is short for English word Diamond Like Carbon, and is a metastable amorphous state film with physical and chemical properties similar to Diamond and unique performance, and the DLC film has the characteristics of high hardness, friction resistance, corrosion resistance, excellent optical transmittance in infrared band and the Like, so that the DLC film becomes an excellent infrared anti-reflection film material. The invention utilizes the DLC film to protect the surface of the window, utilizes the PECVD method to directly deposit the DLC film on the surface of the ZnSe antireflection film, improves the process, ensures that the DLC film can keep good bonding force with a base on the premise of not using any bonding medium or other intermediate layers, and simultaneously reduces the infrared transmittance loss caused by excessive film layers as much as possible.
The present invention decomposes a carbon source gas into various neutral particles (CH) by gas discharge at low pressure3\ CH \ C \ H) and charged particles (CH)5+\CH3+\CH+\H+) The charged particles nucleate and migrate on the surface of the substrate through a series of chemical reactions to grow the DLC film, the plasma promotes the chemical reactions among gases, the temperature (20-200 ℃) required by deposition is reduced, the plasma at low pressure can also promote the diffusion of reactants on the surface of the substrate, the deposition rate is improved, and the particles which are not firmly bonded with the surface of the film layer are etched, so that the bonding force of the film base is enhanced. The film prepared by the plate capacitive coupling radio frequency glow discharge has high deposition rate, compact and uniform film layer and good stability.
In the present invention, the carbon source gas is preferably methane (CH)4) The flow rate of the carbon source gas is preferably 5-100 sccm, more preferably 20-70 sccm, and most preferably 50-70 sccm; the RF power is preferably 100-2500W, more preferably 200-500W, and particularly, in the embodiment of the invention, the RF power can be selected from the range of 100-2500WTo be 200W or 300W; the deposition vacuum degree of the DLC film is preferably 3X 10-3～3×10-5Pa, more preferably 2X 10-3～1×10-4Pa, most preferably 1X 10-3～5×10-4Pa; the deposition temperature is preferably 20-200 ℃, more preferably 30-150 ℃, and most preferably 50-100 ℃, and specifically, in the embodiment of the invention, 180 ℃; the deposition time is preferably 0.1-10 min, more preferably 1-8 min, and most preferably 3-6 min.
In the process of depositing the DLC film, the invention preferably uses argon as a carrier gas, and the flow rate of the argon is preferably 100-200 sccm.
The invention also provides an infrared focal plane array detector with the DLC protective film, which is prepared according to the preparation method and comprises the infrared focal plane array detector and the DLC protective film deposited on the surface of the detector window;
the window of the infrared focal plane array detector takes Ge as a base material and is plated with an antireflection film, and the specific structure is shown in figure 1 and is not repeated herein.
In the invention, the thickness of the DLC protective film is preferably 150-1200 nm; the refractive index of the DLC protective film is preferably 1.8-3.1; the working waveband of the infrared focal plane array detector with the DLC protective film is 3-5 mu m or 8-14 mu m.
The invention provides a preparation method of an infrared focal plane array detector with a DLC protective film, which comprises the following steps: A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution; B) introducing argon into the cleaned window of the infrared focal plane array detector under a vacuum condition, and performing radio frequency plasma cleaning; C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film; the radio frequency power of the step C) is 200-2500W, and the vacuum degree of the step C) is 3 multiplied by 10-3～3×10-5Pa. The invention adopts a radio frequency Plasma Enhanced Chemical Vapor Deposition (PECVD) method on a detectorThe DLC film is deposited on the surface of the window, and meanwhile, the deposition conditions are controlled, so that the DLC film is more uniform in deposition and good in film forming property, and has higher scratch resistance, friction resistance and corrosion resistance while high transmittance and low infrared absorption rate are ensured. In addition, the DLC film has high deposition speed, high single-furnace yield and less damage to the substrate.
The experimental result shows that the detector with the DLC protective film in the invention passes salt spray test (4.5% NaCl, 37 ℃, 96h) and high and low temperature test (-60-70 ℃); the infrared transmittance is between 90 and 97 percent.
In order to further illustrate the present invention, the following detailed description of an infrared focal plane array detector with a DLC protective film and a method for making the same are provided in connection with the examples, which should not be construed as limiting the scope of the present invention.
Example 1
Cleaning a substrate: cleaning with acetone under ultrasound for 5min to remove surface oil stain, cleaning with acetone working solution under ultrasound for 5min, and repeatedly washing with deionized water for 10min to remove surface impurities. Spin-drying in a spin dryer, immediately placing the washed window on a polar plate of a vacuum chamber, and vacuumizing.
Depositing a DLC film: introducing argon when the vacuum degree reaches a set value of 0.0013Pa, regulating the radio frequency power to 300W for argon ion cleaning at the argon flow rate of 30Sccm,
then introducing carbon source gas CH4Setting the radio frequency power at 300W, the chamber temperature at 200 deg.C, the substrate bias voltage at 250v, and the vacuum degree at 3X 10-3Pa, the carbon source gas flow rate was 60sccm, and deposition of a DLC film was started.
And (4) closing the radio frequency power supply after the deposition is finished, stopping introducing the carbon source gas, increasing the flow of the argon gas, releasing vacuum, and taking out the product.
Example 2
Cleaning a substrate: cleaning with acetone under ultrasound for 10min to remove oil stain on the surface, cleaning with acetone working solution under ultrasound for 20min, and repeatedly washing with deionized water for 10min to remove surface impurities. Spin-drying in a spin dryer, immediately placing the washed window on a polar plate of a vacuum chamber, and vacuumizing.
Depositing a DLC film: introducing argon when the vacuum degree reaches a set value of 0.13Pa, adjusting the radio frequency power to 300W for argon ion cleaning at the argon flow rate of 90Sccm,
then introducing carbon source gas CH4Setting RF power at 300W, chamber temperature 175 deg.C, substrate bias voltage, and vacuum degree of 5 × 10-4Pa, the carbon source gas flow rate was 40sccm, and deposition of a DLC film was started.
And (4) closing the radio frequency power supply after the deposition is finished, stopping introducing the carbon source gas, adjusting the flow of the argon gas, releasing the vacuum, and taking out the product.
Example 3
Cleaning a substrate: cleaning with acetone under ultrasound for 10min to remove oil stain on the surface, cleaning with acetone working solution under ultrasound for 10min, and repeatedly washing with deionized water for 10min to remove surface impurities. Spin-drying in a spin dryer, immediately placing the washed window on a polar plate of a vacuum chamber, and vacuumizing.
Depositing a DLC film: introducing argon when the vacuum degree reaches a set value of 0.01Pa, regulating the radio frequency power to 300W for argon ion cleaning at the argon flow rate of 30Sccm,
then introducing carbon source gas CH4Setting RF power at 200W, chamber temperature 175 deg.C, substrate bias, and vacuum degree at 3 × 10-5Pa, the carbon source gas flow rate was 30sccm, and deposition of a DLC film was started.
And (4) closing the radio frequency power supply after the deposition is finished, stopping introducing the carbon source gas, adjusting the flow of the argon gas, releasing the vacuum, and taking out the product.
Comparative example 1
An infrared focal plane array detector having a DLC protective film was produced in the same manner as in example 1, except that the degree of vacuum in the DLC film deposition process in this example was 1 Pa. The power was 200W and the carbon source flow was 20 Sccm.
The probes of examples 1 to 3 and comparative example 1, on which the DLC protective film was deposited, were examined according to the test method of MIL-48616, and the results are shown in Table 1,
TABLE 1 Performance data for the products of inventive examples 1 to 3 and comparative example 1
Adhesion tests were carried out for the DLC film-deposited probes of examples 1 to 3 and comparative example 1 by using a glass tape (1/2' width, type L-T-90 class I). After the adhesive tape was attached to the surface of the film, the glass adhesive tape was rapidly and vertically peeled off, and visual inspection showed that 50% of the products of comparative example 1 were edge-peeled by the adhesion test of the detectors deposited with the DLC protective film of examples 1 to 3.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of an infrared focal plane array detector with a DLC protective film comprises the following steps:
A) cleaning a window of the infrared focal plane array detector by sequentially adopting acetone and working solution;
the window of the infrared focal plane array detector comprises a ZnSe layer, a ZnS layer, a Ge layer, a ZnS layer and a ZnSe layer which are sequentially contacted; the ZnSe layer is in contact with the DLC protective film;
B) introducing argon into the cleaned window of the infrared focal plane array detector under a vacuum condition, and performing radio frequency plasma cleaning; the vacuum degree in the step B) is 0.0013-0.13 Pa;
C) then introducing carbon source gas, and depositing a DLC protective film on the surface of the window of the infrared focal plane array detector by adopting a radio frequency plasma enhanced chemical vapor deposition method to obtain the infrared focal plane array detector with the DLC protective film;
said step C)The radio frequency power of the step (C) is 200-500W, and the vacuum degree of the step (C) is 3 multiplied by 10-3～3×10-5Pa；
The deposition temperature in the step C) is 20-200 ℃; the deposition time in the step C) is 0.1-10 min.
2. The method according to claim 1, wherein the flow rate of argon in step B) is 30 to 90 sccm;
the radio frequency power in the step B) is 300-700W.
3. The production method according to claim 1, wherein the carbon source gas is methane;
the flow rate of the carbon source gas is 5-100 sccm.
4. The method according to claim 1, wherein argon is used as a carrier gas during the deposition of step C);
the flow rate of the argon is 100-200 sccm.
5. The preparation method according to claim 1, wherein the working solution is one or more of acetone, isopropanol and N-methylpyrrolidone.
6. The method for preparing the DLC protective film according to claim 1, wherein the working wavelength band of the infrared focal plane array detector with the DLC protective film is 3-5 μm or 8-14 μm.
7. The method according to claim 1, wherein the DLC protective film has a refractive index of 1.8 to 3.1.
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| CN1020158C (en) * | 1987-12-22 | 1993-03-24 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN101464528B (en) * | 2008-01-23 | 2011-01-12 | 四川大学 | DLC infrared anti-refiection protective film and method for producing the same |
| CN101736313B (en) * | 2008-11-26 | 2011-07-06 | 北京有色金属研究总院 | Method for preparing diamond-like film on germanium substrate |
| CN102997999A (en) * | 2012-11-26 | 2013-03-27 | 烟台睿创微纳技术有限公司 | Infrared focal plane array detector |
| CN106282935A (en) * | 2015-05-15 | 2017-01-04 | 新科实业有限公司 | Material with diamond-like coating and preparation method thereof |
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