CN113013282B - High-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip, preparation method thereof and infrared detector - Google Patents
High-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip, preparation method thereof and infrared detector Download PDFInfo
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Abstract
The invention discloses a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip, a preparation method thereof and an infrared detector, wherein the preparation of the chip comprises the following steps: preparing a buffer layer and C on a chip substrate 60 A thin film, pbSe thin film; sensitizing the PbSe film; in PbSe thin films and C 60 And preparing an electrode on the film. The preparation method has the advantages of simple process, convenient operation, low cost and the like, and the prepared infrared detection chip has the advantages of small size, large array, large scale, quick response, high responsiveness, high sensitivity and the like, and has very important significance for expanding the application range of the infrared detector. The infrared detector takes the chip as a core element of the detector, can meet the requirements of short response time, high sensitivity and the like, and has simple preparation process without refrigeration; meanwhile, the reference detector is arranged, so that the detection sensitivity and the detection reliability can be improved.
Description
Technical Field
The invention belongs to the technical field of infrared detector preparation, and relates to a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip, a preparation method thereof and an infrared detector.
Background
The infrared detector is a photoelectric device for converting infrared radiation into electronic signals, wherein photoelectric reaction is only carried out on a photosensitive element, and subsequent signal processing steps only involve electronics, so that an infrared detection chip is a core element of the infrared detector.
Compared with a pyroelectric detector and a thermopile detector, the photoelectric detector has the advantages of high response speed, high responsivity, high sensitivity and the like. The market has a strong demand for uncooled Photovoltaic (PV) detectors in the mid-Infrared (IR) wavelength range, which have no cooling system, are inexpensive, and are much smaller than the refrigerated detectors.
Auger recombination is a main loss channel of the conventional semiconductor mid-infrared detector at high temperature, and is a key obstacle for the development of the conventional semiconductor mid-infrared detector. However, the advantages of such low auger recombination have not been fully explored in the context of lead salt photovoltaic detectors, in part due to the lack of good binding of low dark current. Therefore, finding a suitable semiconductor material to form a good heterojunction with Pb-salts is critical to the device.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip with simple process, convenient operation and low cost, a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip with small size, large array, large scale, quick response, high responsivity and high sensitivity prepared by the preparation method, and an infrared detector comprising the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip comprises the following steps:
s1, preparing a buffer layer on a chip substrate;
s2, preparing C on the buffer layer prepared in the step S1 by adopting an evaporation process 60 A film;
s3, adopting ion beam sputtering technology to prepare C in the step S2 60 Preparing a PbSe film on the film;
s4, sensitizing the PbSe film prepared in the step S3;
s5, after the sensitization treatment of the step S4 is finished, a PbSe thin film and C are added 60 And preparing an electrode on the film to obtain the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip.
In the step S3, the parameters of the ion beam sputtering process in the preparation process of the PbSe thin film are as follows: the sputtering voltage is 200V-400V, and the sputtering current is 25A-40A; the film forming speed of the PbSe film is 2 nm/min-4 nm/min.
In the above preparation method, further improvement is provided, in the step S3, the thickness of the PbSe thin film is 500nm to 2 μm.
In the above preparation method, it is further improved that, in the step S3, the preparation process of the PbSe thin film further includes doping the PbSe thin film; the element doped In the doping treatment process is at least one of Te, cd, in and Sr.
In the above preparation method, it is further improved that in the step S1, the chip substrate is glass or a silicon wafer; the buffer layer is CaF 2 、BaF 2 、Si 3 N 4 At least one of; the thickness of the buffer layer is 5 nm-20 nm.
In the above preparation method, further improvement is that in the step S2, the step C 60 The technological parameters of the evaporation process in the preparation process of the film are as follows: the temperature is 550-700 ℃, and the vacuum degree is 10 -4 Pa is above; said C is 60 The film forming rate of the film is 3A/s-5A/s; said C is 60 The thickness of the film is 40 nm-200 nm.
In the step S4, the sensitization treatment is performed by heat treatment at 150-400 ℃ for 10-30 min under oxygen atmosphere, and then at I 2 Heat treatment is carried out for 2min to 6min at the temperature of 150 ℃ to 400 ℃ under the steam atmosphere.
As a general technical concept, the invention also provides a high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip prepared by the preparation method.
In the high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip, the chip is further improved, and comprises a chip substrate; a buffer layer is arranged on the chip substrate; the buffer layer is provided with a C 60 A film; said C is 60 The film is provided with a PbSe film and an electrode; and an electrode is arranged on the PbSe film.
As a general technical concept, the present invention also provides an infrared detector including a measurement detector and a reference detector; the measurement detector and the reference detector both comprise the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip; and the front end of the sensing surface of the infrared detector is provided with an optical filter.
Compared with the prior art, the invention has the advantages that:
(1) The invention provides a preparation method of a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip, which comprises the following steps: preparing a buffer layer on a chip substrate; preparing C on the buffer layer by adopting an evaporation process 60 A film; using ion beam sputtering process at C 60 Preparing a PbSe film on the film; sensitizing the PbSe film; after sensitization, in the buffer layer and C 60 And preparing an electrode on the film to obtain the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip. In the invention, the ion beam sputtering process is adopted to prepare the PbSe film on the buffer layer, so that the bonding strength and the crystallization property of the PbSe film and a matrix can be improved, the PbSe film has the advantages of high bonding strength with the matrix, good crystallization property and the like, the dark current of a detection chip can be reduced, and the infrared light response of the detection chip is improvedDegree, response speed, and detection sensitivity; the PbSe film prepared by the process has small size, is beneficial to realizing the miniaturized design and preparation of the detection chip, and can realize the preparation of a large-array large-scale detector through the improvement of proper process equipment; meanwhile, the ion beam sputtering process is simpler and more convenient to operate, the preparation of the uncooled PbSe film can be realized, and the preparation cost of the PbSe film can be reduced, so that the manufacturing and using cost of the detection chip can be further reduced. In the invention, the PbSe film is sensitized, so that the photoelectric property can be further improved. The preparation method has the advantages of simple process, convenient operation, low cost and the like, and the prepared high-response PbSe/C60 heterojunction photosensitive film infrared detection chip has the advantages of small size, large array, large scale, quick response, high responsiveness, high sensitivity and the like, and has very important significance for expanding the application range of the infrared detector.
(2) In the preparation method of the invention, C is optimized 60 Preparation process of film, adopting evaporation process to prepare C 60 The film, and optimized the technological parameter of coating by vaporization technology, specific: the temperature is 550-700 ℃, and the vacuum degree is 10 -4 The film forming rate of the C60 film is 3A/s-5A/s by Pa or above, and is regulated to 3A/s-5A/s by controlling the temperature to be 550-700 ℃, so that the evaporation efficiency can be improved, and the C can be improved 60 The uniformity of the film was further controlled by controlling the degree of vacuum to 10 -4 Pa above is beneficial to realizing the control of the temperature to the film deposition rate, otherwise, the evaporation temperature can be increased to reach the required rate, and the service life of the evaporation equipment is reduced.
(3) In the preparation method, the lead selenide is brittle, so that the parameters of an ion beam sputtering process in the preparation process of the PbSe film are optimized, the sputtering voltage is optimized to 200V-400V, the sputtering current is optimized to 25A-40A, the sputtering power range is controlled not to be too high, the uniformity of film forming is facilitated under the sputtering power condition, and the faster film forming speed can be ensured; meanwhile, under the condition, the preparation of the PbSe film with high bonding strength with a substrate and good crystallization performance is more favorable, so that the dark current of a detection chip is further reduced, and the infrared light responsivity, the response speed and the detection sensitivity of the detection chip are further improved.
(4) In the preparation method, the conditions of sensitization treatment are optimized, and the preparation method specifically comprises the following steps: firstly, heat treatment is carried out for 10min to 30min at the temperature of 150 ℃ to 400 ℃ under the oxygen atmosphere, and then the mixture is heated at the temperature of I 2 The PbSe film prepared by the ion sputtering process has a plurality of defects, such as Pb vacancies and Se interstitial atoms, which can be eliminated by the recrystallization process in the high-temperature heat treatment, but the atmosphere, the temperature and the time in the heat treatment process can influence the recrystallization; in an oxygen atmosphere, oxygen can rapidly react with Pb vacancies and Se interstitials, and if the heat treatment time is too long, pbSe is easily deviated from the stoichiometric ratio seriously due to excessive reaction of the defects and oxygen, and PbSe is formed on the surface of the film layer or in the interstitials of the crystal grains 1-x O x Even PbO layer, and if the time is too short, the situation that PbSe is not oxidized or the oxidation degree is lower easily occurs; if the heat treatment temperature is too low, oxygen cannot be promoted to oxidize with PbSe in the heat treatment process, so that the film layer does not show photoelectric property, and if the temperature is too high, a thick oxide layer can be formed on the surface of the PbSe film, so that the resistance value of the film layer is increased, the carrier concentration is further reduced, and the change of the photoelectric property is not facilitated, so that the time and the temperature of the oxygen treatment need to be properly controlled. I is 2 Can activate the photosensitive property of PbSe, and promote the activation of PbSe by breaking larger micro grains into smaller microcrystalsCoalescence between PbSe crystals is realized, so that the surface is smoother; at the same time, the resistance of the film is further increased, which has a critical effect on the sensitization of PbSe, so that the heat treatment conditions under iodine vapor are also controlled to control I 2 In the case of PbSe aggregation, i.e. in contact with PbSe is minimized 2 The content is reduced to the minimum to ensure effective activation under the iodine vapor atmosphere and improve the photosensitive property of PbSe, because iodine has strong oxidation effect, if the time is too long, I2 reacts with PbSe to generate more iodide, the substance is easy to gather on the surface of the PbSe film to influence light absorption, and if the amount is too small, the oxidation effect is not good. In the invention, the detection rate of the infrared detector consisting of the prepared lead selenide film can reach 5 multiplied by 10 8 ~2.5×10 10 cm·Hz 1/2 ·W -1 Compared with the conventional photoconductive detector adopting the conventional sensitization treatment process, the photoconductive detector is higher by more than 1-2 orders of magnitude.
(5) The invention provides a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip which comprises a chip substrate, wherein a buffer layer is arranged on the chip substrate, and a C layer is arranged on the buffer layer 60 Film, C 60 The film is provided with a PbSe film and an electrode, and the PbSe film is provided with the electrode. In the high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip, C 60 Forms a heterojunction with PbSe having a band gap, and incident photons generate electron-hole pairs in PbSe, and then the holes are transferred to C 60 Channel drift toward drain, electrons remain in PbSe, and (recycled) carriers exist in C for a long time through capacitive coupling 60 In the channel, a photovoltaic effect is generated, the light responsivity of the detection chip can be improved by utilizing the photovoltaic principle, the infrared detection is realized, and the infrared detection chip is formed. The high-response PbSe/C60 heterojunction photosensitive film infrared detection chip has the advantages of small size, large array scale, high response speed, high responsivity, high sensitivity and the like, and has high use value and good application prospect.
(6) The invention provides an infrared detector, which comprises a high-response PbSe/C60 heterojunction photosensitive film infrared detection chip, wherein the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip is taken as a core element of the detector, so that the infrared detector can meet the requirements of short response time, high sensitivity and the like, the preparation process is simple, and refrigeration is not needed; meanwhile, by arranging the reference detector, the influence of unstable factors on the measurement result can be eliminated, and the detection sensitivity and the detection reliability can be improved. The infrared detector can accurately detect hazardous gases such as methane in urban environment, such as natural gas leakage, and eliminate potential safety hazards in time; such as air detection, the method is also of great significance for real-time monitoring of carbon dioxide, carbon monoxide, ammonia gas and hydrogen sulfide (smelling of rotten eggs).
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
FIG. 1 is a flow chart of a process for preparing a high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip in example 1 of the present invention.
FIG. 2 is a schematic structural diagram of a high-response PbSe/C60 heterojunction photosensitive thin-film infrared detection chip in embodiment 1 of the invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
Example 1
A preparation method of a high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip is shown in a flow chart of a preparation process of the chip in figure 1 and comprises the following steps:
(1) Cleaning the substrate, and vapor-depositing a buffer layer (specifically CaF) on the substrate (specifically silicon wafer) 2 ) And the thickness is 10nm. The buffer layer material adopted in the invention can increase the transmission, because CaF 2 Lattice-matched to Si (Δ a/a = 0.6%), and has the same coefficient of thermal expansion as PbSe (CaF) 2 Is 19.1 x 10 6 K -1 And PbSe is 19.4 x 10 6 K -1 ) Thus CaF 2 Can well relieve the mismatching between Si and PbSe and is beneficial to obtaining a high-quality PbSe film.
(2) Preparing C on the buffer layer prepared in the step (1) by adopting an evaporation process 60 Film with thickness of 60nm, wherein the temperature is controlled at 650 deg.C and vacuum degree is 10 -4 Pa or more, C 60 The film formation rate of the thin film was 5A/s.
(3) C prepared in step (2) by adopting ion beam sputtering method 60 Preparing a PbSe film on the film, wherein the thickness of the film is 1 mu m, the sputtering voltage is 400V, the sputtering current is 35A, and the film forming rate of the PbSe film is 3nm/min; meanwhile, cd element is doped into the PbSe film in an ion implantation mode in the preparation process of the PbSe film, and the forbidden bandwidth is adjusted by doping the Cd element, so that the absorption of infrared optics in a waveband of 2.6-4.2 mu m is realized.
(4) And (4) placing the PbSe film prepared in the step (3) in an oxygen atmosphere, carrying out heat treatment at 360 ℃ for 20min, then placing the PbSe film in an iodine vapor atmosphere, and carrying out heat treatment at 360 ℃ for 2min to complete sensitization treatment on the PbSe film.
(5) After the sensitization treatment in the step (4) is finished, processes such as photoetching, developing, film coating, photoresist removing and the like (such as photoetching of a contact electrode Au pattern and preparation of an electrode Au by ion beam sputtering) are adopted to sensitize the PbSe film and the C 60 And preparing a gold electrode on the film to obtain the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip.
The high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip prepared in the embodiment comprises a chip substrate, wherein a buffer layer is arranged on the chip substrate, and a C layer is arranged on the buffer layer, as shown in FIG. 2 60 Film, C 60 The film is provided with a PbSe film and a gold electrode, and the PbSe film is provided with a gold electrode.
An infrared detector comprises a measurement detector and a reference detector, wherein the measurement detector and the reference detector both comprise the high-response PbSe/C60 heterojunction photosensitive thin-film infrared detection chip prepared in the embodiment 1. In the infrared detector, the front ends of the sensing surfaces of the measurement detector and the reference detector are provided with the optical filter, and the structural design of the optical filter replaces a filter circuit in the traditional detector, so that the power consumption of the detector is further reduced.
In this embodiment, the infrared detector has a dual-chip structure, and its detection principle specifically is: the infrared radiation of the light source respectively reaches a reference detector and a measuring detector after being absorbed by the mixed gas, wherein the measuring detector measures the infrared intensity absorbed by the target gas, the reference detector measures the infrared intensity not absorbed, the radiation energy which is received by the measuring detector when the target gas does not exist can be obtained through the radiation intensity information measured by the reference detector and the light-emitting characteristic of the light source, and the difference value of the actual measurement values of the reference detector and the measuring detector is the absorption capacity of the target gas to the infrared radiation. The differential measurement method of the infrared detector can eliminate the influence of factors such as unstable power of the light source and the like on the measurement result, and improve the detection sensitivity and the detection reliability.
In this embodiment, the infrared detector can achieve the following technical indexes:
spectral response range: 2.6-4.0 μm
Detection rate: 9X 10 8 cm·Hz 1/2 ·W -1
Response time: less than or equal to 1 mu s;
working temperature: 0-60 ℃.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (7)
1. A preparation method of a high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip is characterized by comprising the following steps:
s1, preparing a buffer layer on a chip substrate;
s2, preparing C on the buffer layer prepared in the step S1 by adopting an evaporation process 60 A film; said C is 60 The technological parameters of the evaporation process in the preparation process of the film are as follows: the temperature is 550-700 ℃, and the vacuum degree is 10 -4 Pa is above; said C is 60 The film forming rate of the film is 3A/s-5A/s; said C is 60 The thickness of the film is 40 nm-200 nm;
s3, adopting ion beam sputtering technology to prepare C in the step S2 60 Preparing a PbSe film on the film; the parameters of the ion beam sputtering process in the preparation process of the PbSe film are as follows: the sputtering voltage is 200V-400V, and the sputtering current is 25A-40A; the film forming speed of the PbSe film is 2 nm/min-4 nm/min; the thickness of the PbSe film is 500 nm-2 mu m;
s4, sensitizing the PbSe film prepared in the step S3;
s5, after the sensitization treatment in the step S4 is finished, the PbSe thin film and C are added 60 And preparing an electrode on the film to obtain the high-response PbSe/C60 heterojunction photosensitive film infrared detection chip.
2. The preparation method according to claim 1, wherein in the step S3, the preparation process of the PbSe thin film further comprises doping the PbSe thin film; the element doped In the doping treatment process is at least one of Te, cd, in and Sr.
3. The production method according to claim 1 or 2, wherein in the step S1, the chip substrate is a glass or silicon wafer; the buffer layer is CaF 2 、BaF 2 、Si 3 N 4 At least one of (a); the thickness of the buffer layer is 5 nm-20 nm.
4. The method according to claim 1 or 2, wherein in the step S4, the sensitization treatment is a heat treatment under an oxygen atmosphere at 150 to 400 ℃ for 10 to 30min, and then I 2 Heat treatment is carried out for 2min to 6min at the temperature of 150 ℃ to 400 ℃ under the steam atmosphere.
5. A high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip, which is prepared by the preparation method of any one of claims 1 to 4.
6. The high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip according to claim 5, wherein the high-response PbSe/C60 heterojunction photosensitive thin film infrared detection chip comprises a chip substrate; a buffer layer is arranged on the chip substrate; the buffer layer is provided with a C 60 A film; said C is 60 The film is provided with a PbSe film and an electrode; an electrode is arranged on the PbSe thin film; the electrode is a gold electrode.
7. An infrared detector is characterized by comprising a measurement detector and a reference detector; the high-response PbSe/C60 heterojunction photosensitive thin-film infrared detection chip as claimed in claim 5 or 6 is included in each of the measurement detector and the reference detector; and the front end of the sensing surface of the infrared detector is provided with an optical filter.
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