CN109659396B - Preparation method of intermediate infrared transparent P-type semiconductor film - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004065 semiconductor Substances 0.000 title claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 21
- 239000013077 target material Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 15
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 63
- 239000010453 quartz Substances 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000011248 coating agent Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 22
- 229910052594 sapphire Inorganic materials 0.000 claims description 18
- 239000010980 sapphire Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 239000012494 Quartz wool Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007888 film coating Substances 0.000 claims description 4
- 238000009501 film coating Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000002834 transmittance Methods 0.000 abstract description 9
- 239000004020 conductor Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 19
- 238000012360 testing method Methods 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
A preparation method of a middle infrared transparent P-type semiconductor film relates to a preparation method of a P-type semiconductor film. The invention aims to develop a novel P-type intermediate infrared transparent conductive material variety and solve the problem of the existing LaSe2The preparation of the film mid-infrared transparent conductive film is difficult, and the application in mid-infrared is greatly limited. The invention comprises the following steps: firstly, cleaning a target material and a substrate; II, La2O3Preparing a film; III, LaSe2And (3) preparing a film. The invention takes simple substance Se powder as a Se source, utilizes vacuum tube sealing treatment, and Se vapor can react La with the Se vapor under the condition of selenizing annealing2O3Preparation of LaSe by using principle of replacing O in film2The film makes up the limitation of the preparation of materials which are not easy to react at higher temperature of La and Se. LaSe prepared by the invention2The film has good conductivity, the total transmittance of the medium-wave infrared region is about 70%, and the transmittance is good.
Description
Technical Field
The invention relates to a preparation method of a P-type semiconductor film.
Background
The light sensor plays a role in daily lifeThe realization of the functions of signal tracking, light sensing imaging and the like in the fields of military equipment, artificial intelligence and the like, which are lacking in roles, needs the participation of a light sensing detector. However, the intensity of the external electromagnetic wave and the light source signal can seriously affect the working effect of the detector, so that the detection signal of the detector is weakened, the imaging quality has larger deviation with an actual object, and even effective imaging and information feedback cannot be realized. In order to reduce the interference of external signals such as electromagnetic waves, Transparent Conductive Films (TCFs) generally need to be plated on the detector window, so that the detector window has both excellent optical transparency and strong electromagnetic shielding performance. However, conventional N-type TCFs represented by Indium Tin Oxide (ITO) have good visible light transmittance (c:)>85%) and superior electrical properties (carrier concentration: 1018～1021cm-3(ii) a Mobility: 5-100 cm2·V-1·s-1) However, the transmission of N-type TCFs in the infrared band (1-12 μm) cannot be realized. The wavelength of traditional N-type TCFs plasma is adjusted by adjusting and controlling electrical parameters such as carrier concentration of the film, the transmission performance of the film in a near infrared band can be realized furthest, the film cannot extend to a middle infrared (3-5 mu m) or even a long-wave infrared region (8-12 mu m), and the application range of devices such as a light sensitive detector and the like is limited by the N-type TCFs. Nowadays, the light-sensitive detector is developing towards all-weather high-sensitivity direction, and generally needs to have dual-purpose ability of day and night, and the ability of adapting to complex electromagnetic interference signal environment and detecting weak signals, so that the realization of excellent middle and long infrared band transparent conductive characteristics by TCFs is very important. The conventional intermediate infrared band transparent conductive material is intrinsic P type CuAlO with a delafossite structure2And with Cu+Oxides of the structure of the basic series delafossite (CuMO)2P-type TCFs of this type have good mid-infrared transmission performance (75%) but have low hole concentrations (1.3 × 10)17cm-3) And excellent conductivity cannot be realized, so that the light-sensitive detector is greatly influenced in the aspect of electromagnetic interference. LaSe2The film is a potential mid-infrared transparent conductive film, but conventional La and Se react with each other to prepare LaSe2Thin films are very difficult, thus also making LaSe2The preparation of thin films and mid-infrared applications are greatly limited.
Disclosure of Invention
The invention aims to solve the problem of the existing LaSe2The preparation of the film is very difficult, and the application of the mid-infrared is greatly limited, so that the preparation method of the mid-infrared transparent P-type semiconductor film is provided.
The preparation method of the intermediate infrared transparent P-type semiconductor film is carried out according to the following steps:
firstly, cleaning a target material and a substrate:
under the condition that the ultrasonic power is 100W-300W, sequentially placing the metal La target material in acetone, alcohol and deionized water to be respectively cleaned for 20 min-30 min to obtain a clean La target material;
under the condition that the ultrasonic power is 50W-200W, sequentially placing sapphire sheets with the size of 10mm × 10mm × 1mm in acetone, alcohol and deionized water for respectively cleaning for 10 min-20 min to obtain clean sapphire substrate materials;
II, La2O3Preparing a film:
①, preparing before film coating, installing clean La target material and clean sapphire substrate material, starting the device to vacuumize to the air pressure of 6 × 10-5Pa～4×10-5Pa；
②, coating film, introducing Ar and O2When the pressure is 0.5Pa to 0.6Pa, the coating power supply is a radio frequency power supply, the coating power is 50W to 55W, the pre-sputtering is carried out for 5min to 10min under the condition of the pressure of 0.5Pa to 0.6Pa, the target baffle is opened, and the sputtering coating is carried out for 60min to 65min under the condition of the pressure of 0.5Pa to 0.6 Pa; the flow rate of Ar is 20sccm and O2The flow rate of (3 sccm);
③, shutting down the machine, closing all power supplies, opening the air release valve, deflating and opening the bin, and taking out the sample to be the La2O3Film, now La plated2O3The thickness of the film is 190 nm-210 nm;
III, LaSe2Preparing a film:
①, weighing Se powder with the mass of 0.01 g-0.05 g, putting the Se powder into a No. 1 quartz tube with the diameter of 10mm and the length of 10cm and with a single end opening, and sealing the single end opening by quartz wool;
②, respectively coating La prepared in the second step2O3The sapphire sheet of the thin film and the quartz tube No. 1 containing Se powder in the step III ① were put into a quartz tube No. 2 having a diameter of 18mm and a length of 20cm and having a single end opened, and then the quartz tube No. 2 was evacuated to a vacuum pressure of 5 × 10-3Pa～2×10-3After Pa, the single end opening of No. 2 quartz tube is sealed, so that La2O3The film and the No. 1 quartz tube filled with Se powder are jointly in a sealed vacuum environment;
③, placing the vacuum sealed No. 2 quartz tube into a tube furnace for annealing treatment, wherein the annealing temperature is 600-1000 ℃, the annealing time is 0.5-4 h, and the heating rate of the tube furnace is 3-5 ℃/min;
④, naturally cooling the tube furnace to room temperature, opening the tube furnace and taking out a sample to obtain LaSe2A film.
The invention takes simple substance Se powder as a Se source, utilizes vacuum tube sealing treatment, and Se vapor can react La with the Se vapor under the condition of selenizing annealing2O3Preparation of LaSe by using principle of replacing O in film2The film makes up the limitation of the preparation of materials which are not easy to react at higher temperature of La and Se.
The invention has the beneficial effects that:
the invention adopts a simple method to prepare LaSe2The P-type TCFs film combines a magnetron sputtering coating system and a selenization annealing mode to prepare LaSe2The film cost is low, and the process operation is simple;
LaSe prepared by the invention2The film has better conductivity, and the maximum concentration of the current carrier can reach 1019cm-3The conductivity can reach 3.69S/m by the order of magnitude; the P-type TCFs film is plated on a sapphire substrate, the total transmittance of a medium-wave infrared region is about 70%, and the transmittance performance is good. P-type LaSe2The discovery of the thin film material widens the material selection range of the current P-type TCFs materialThe method is beneficial to promoting the research of related mid-infrared transparent devices and the like.
Drawings
FIG. 1 is an XRD pattern;
FIG. 2 is LaSe2A test curve graph of the medium wave infrared transmittance of the film;
FIG. 3 is LaSe2Graph for testing electrical properties of the film.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a mid-infrared transparent P-type semiconductor film, which is specifically carried out according to the following steps:
firstly, cleaning a target material and a substrate:
under the condition that the ultrasonic power is 100W-300W, sequentially placing the metal La target material in acetone, alcohol and deionized water to be respectively cleaned for 20 min-30 min to obtain a clean La target material;
under the condition that the ultrasonic power is 50W-200W, sequentially placing sapphire sheets with the size of 10mm × 10mm × 1mm in acetone, alcohol and deionized water for respectively cleaning for 10 min-20 min to obtain clean sapphire substrate materials;
II, La2O3Preparing a film:
①, preparing before film coating, installing clean La target material and clean sapphire substrate material, starting the device to vacuumize to the air pressure of 6 × 10-5Pa～4×10-5Pa；
②, coating film, introducing Ar and O2When the pressure is 0.5Pa to 0.6Pa, the coating power supply is a radio frequency power supply, the coating power is 50W to 55W, the pre-sputtering is carried out for 5min to 10min under the condition of the pressure of 0.5Pa to 0.6Pa, the target baffle is opened, and the sputtering coating is carried out for 60min to 65min under the condition of the pressure of 0.5Pa to 0.6 Pa; the flow rate of Ar is 20sccm and O2The flow rate of (3 sccm);
③, shutting down the machine, closing all power supplies, opening the air release valve, deflating and opening the bin, and taking out the sample to be the La2O3Film, now La plated2O3The thickness of the film is 190 nm-210 nm;
III, LaSe2Preparation of films：
①, weighing Se powder with the mass of 0.01 g-0.05 g, putting the Se powder into a No. 1 quartz tube with the diameter of 10mm and the length of 10cm and with a single end opening, and sealing the single end opening by quartz wool;
②, respectively coating La prepared in the second step2O3The sapphire sheet of the thin film and the quartz tube No. 1 containing Se powder in the step III ① were put into a quartz tube No. 2 having a diameter of 18mm and a length of 20cm and having a single end opened, and then the quartz tube No. 2 was evacuated to a vacuum pressure of 5 × 10-3Pa～2×10-3After Pa, the single end opening of No. 2 quartz tube is sealed, so that La2O3The film and the No. 1 quartz tube filled with Se powder are jointly in a sealed vacuum environment;
③, placing the vacuum sealed No. 2 quartz tube into a tube furnace for annealing treatment, wherein the annealing temperature is 600-1000 ℃, the annealing time is 0.5-4 h, and the heating rate of the tube furnace is 3-5 ℃/min;
④, naturally cooling the tube furnace to room temperature, opening the tube furnace and taking out a sample to obtain LaSe2A film.
Second embodiment the difference between the first embodiment and the second embodiment is that step two ① is performed by installing a clean La target and a clean sapphire substrate, and opening the apparatus to vacuum to a pressure of 6 × 10-5Pa. The rest is the same as the first embodiment.
Third embodiment different from the first or second embodiment in that Ar and O are introduced into the second step ②2To a pressure of 0.5 Pa. The others are the same as in the first or second embodiment.
Fourth embodiment, this embodiment is different from the first to third embodiments in that the sputtering coating is performed for 60min under the pressure of 0.5Pa in the second ②.
Fifth embodiment fifth, the present embodiment is different from the fourth embodiment in that the temperature increase rate of the tube furnace in the third ③ step is 5 ℃/min.
The invention was verified with the following tests:
test one: the test is a preparation method of a middle infrared transparent P-type semiconductor film, and is specifically carried out according to the following steps:
firstly, cleaning a target material and a substrate:
sequentially placing the metal La target material in acetone, alcohol and deionized water to be respectively cleaned for 20min under the condition that the ultrasonic power is 100W, so as to obtain a clean La target material;
under the condition that the ultrasonic power is 100W, sequentially placing sapphire sheets with the size of 10mm × 10mm and the size of 10mm × 1mm in acetone, alcohol and deionized water, and respectively cleaning for 10min to obtain a clean sapphire substrate material;
II, La2O3Preparing a film:
①, preparing before film coating, installing clean La target material and clean sapphire substrate material, starting the device to vacuumize to the air pressure of 6 × 10-5Pa；
②, coating film, introducing Ar and O2When the pressure is 0.5Pa, the coating power supply is a radio frequency power supply, the coating power is 50W, the target material baffle is opened for sputtering for 5min under the condition of the pressure of 0.5Pa, and the coating is carried out for 60min under the condition of the pressure of 0.5 Pa; the flow rate of Ar is 20sccm and O2The flow rate of (3 sccm);
③, shutting down the machine, closing all power supplies, opening the air release valve, deflating and opening the bin, and taking out the sample to be the La2O3Film, now La plated2O3The thickness of the film is 200 nm;
III, LaSe2Preparing a film:
①, weighing Se powder with the mass of 0.03g, putting the Se powder into a No. 1 quartz tube with the diameter of 10mm and the length of 10cm and with a single end open, and sealing the single end open with quartz wool;
②, respectively coating La prepared in the second step2O3The sapphire sheet of the thin film and the quartz tube No. 1 containing Se powder in the step III ① were put into a quartz tube No. 2 having a diameter of 18mm and a length of 20cm and having a single end opened, and then the quartz tube No. 2 was evacuated to a vacuum pressure of 3 × 10-3After Pa, a No. 2 quartz tube is put inSealing the tube at the single end of La2O3The film and the No. 1 quartz tube filled with Se powder are jointly in a sealed vacuum environment;
③, placing the vacuum sealed No. 2 quartz tube into a tube furnace for annealing treatment, wherein the annealing temperature is 800 ℃, the annealing time is 1h, and the heating rate of the tube furnace is 5 ℃/min;
④, naturally cooling the tube furnace to room temperature, opening the tube furnace and taking out a sample to obtain LaSe2A film.
FIG. 1 is an XRD pattern with LaSe prepared in run one above2Film, under which is monoclinic phase LaSe2PDF #75-2270 curves, as can be seen from FIG. 1, the film prepared in one experiment is monoclinic phase LaSe2。
Experiment two this experiment was different from experiment one in that the annealing temperature in step three ③ was 600 c, and the others were the same as experiment one.
Experiment three this experiment was different from experiment one in that the annealing temperature in step three ③ was 700 c, and the others were the same as experiment one.
Experiment four this experiment differs from experiment one in that the annealing temperature in step three ③ was 900 c, otherwise the same as experiment one.
Experiment five this experiment was different from experiment one in that the annealing temperature in step three ③ was 1000 c, and the others were the same as experiment one.
FIG. 2 is LaSe2The middle wave infrared transmittance test curve of the film, curve a is LaSe prepared by experiment two2Film, Curve b test three prepared LaSe2Film, Curve c LaSe prepared in experiment one2Thin films, as can be seen in the figure, LaSe increases with the selenization annealing temperature2The film exhibits a tendency to increase and then decrease in mid-wave infrared transmittance, with the highest transmittance being about 78% at 700 ℃.
FIG. 3 is LaSe2The electrical property test curve of the film, curve 1 is the carrier concentration curve, curve 2 is the conductivity curve, it can be seen from figure 3 that the electrical property of the film shows the trend of increasing first and then decreasing with the increase of the selenization annealing temperature, and the electrical property test curve of the film is shown in figure 3When the film is annealed at 800 ℃, the film has the best electrical property, and the current carrier concentration of the film reaches 1.179 × 1019cm-3The conductivity was 3.69S/cm.
Claims (1)
1. A preparation method of a mid-infrared transparent P-type semiconductor film is characterized by comprising the following steps:
firstly, cleaning a target material and a substrate:
sequentially placing the metal La target material in acetone, alcohol and deionized water to be respectively cleaned for 20min under the condition that the ultrasonic power is 100W, so as to obtain a clean La target material;
under the condition that the ultrasonic power is 100W, sequentially placing sapphire sheets with the size of 10mm × 10mm and the size of 10mm × 1mm in acetone, alcohol and deionized water, and respectively cleaning for 10min to obtain a clean sapphire substrate material;
II, La2O3Preparing a film:
①, preparing before film coating, installing clean La target material and clean sapphire substrate material, starting the device to vacuumize to the air pressure of 6 × 10-5Pa；
②, coating film, introducing Ar and O2When the pressure is 0.5Pa, the coating power supply is a radio frequency power supply, the coating power is 50W, the target material baffle is opened for sputtering for 5min under the condition of the pressure of 0.5Pa, and the coating is carried out for 60min under the condition of the pressure of 0.5 Pa; the flow rate of Ar is 20sccm and O2The flow rate of (3 sccm);
③, shutting down the machine, closing all power supplies, opening the air release valve, deflating and opening the bin, and taking out the sample to be the La2O3Film, now La plated2O3The thickness of the film is 200 nm;
III, LaSe2Preparing a film:
①, weighing Se powder with the mass of 0.03g, putting the Se powder into a No. 1 quartz tube with the diameter of 10mm and the length of 10cm and with a single end open, and sealing the single end open with quartz wool;
②, respectively coating La prepared in the second step2O3Sapphire sheet of thin film andthe No. 1 quartz tube filled with the Se powder in the step three ① is placed in a No. 2 quartz tube with a single end opening and the diameter of 18mm and the length of 20cm, and then the No. 2 quartz tube is vacuumized to the pressure of 3 × 10-3After Pa, the single end opening of No. 2 quartz tube is sealed, so that La2O3The film and the No. 1 quartz tube filled with Se powder are jointly in a sealed vacuum environment;
③, placing the vacuum sealed No. 2 quartz tube into a tube furnace for annealing treatment, wherein the annealing temperature is 800 ℃, the annealing time is 1h, and the heating rate of the tube furnace is 5 ℃/min;
④, naturally cooling the tube furnace to room temperature, opening the tube furnace and taking out a sample to obtain LaSe2A film;
the LaSe2The film had a carrier concentration of 1.179 × 1019cm-3The conductivity was 3.69S/cm.
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| CN105063565A (en) * | 2015-08-31 | 2015-11-18 | 哈尔滨工业大学 | Method for preparing P-type infrared transparent conductive oxide film |
| CN108149210A (en) * | 2017-12-26 | 2018-06-12 | 哈尔滨工业大学 | A kind of preparation method of LONG WAVE INFRARED anti-reflection protective film |
| CN108470782A (en) * | 2018-03-09 | 2018-08-31 | 哈尔滨工业大学 | A kind of middle infrared transparent conductive p-type oxide film material and preparation method thereof |
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| CN105063565A (en) * | 2015-08-31 | 2015-11-18 | 哈尔滨工业大学 | Method for preparing P-type infrared transparent conductive oxide film |
| CN108149210A (en) * | 2017-12-26 | 2018-06-12 | 哈尔滨工业大学 | A kind of preparation method of LONG WAVE INFRARED anti-reflection protective film |
| CN108470782A (en) * | 2018-03-09 | 2018-08-31 | 哈尔滨工业大学 | A kind of middle infrared transparent conductive p-type oxide film material and preparation method thereof |
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