CN115000230B - TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with vertical structure and preparation method thereof - Google Patents
TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with vertical structure and preparation method thereof Download PDFInfo
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 99
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0312—Inorganic materials including, apart from doping materials or other impurities, only AIVBIV compounds, e.g. SiC
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
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Abstract
The invention belongs to the field of semiconductor photodetectors, and discloses a TiN enhanced 4H-SiC-based broad spectrum photodetector with a vertical structure and a preparation method thereof, wherein the preparation method comprises the following steps: a top electrode layer, a TiN-NCCs layer, a semiconductor layer and Al which are sequentially arranged from top to bottom 2 O 3 The top electrode layer is a semitransparent metal electrode, the TiN-NCCs layer is a TiN nanometer concave-convex structure, the semiconductor layer is a 4H-SiC substrate, and the bottom electrode layer is an opaque metal electrode. The invention respectively arranges the top electrode and the bottom electrode at two sides of the 4H-SiC semiconductor layer to form a photoelectric detector with a vertical structure, and the bright current of the device in a wide spectrum range is increased by introducing TiN nano particles at the interface of the 4H-SiC semiconductor layer and the top electrode layer, and in addition, 0.6nm Al is introduced 2 O 3 The layer is used as a modification layer, so that dark current rise of the device caused by introducing TiN-NCCs can be restrained, and the performance of the wide-spectrum detector is improved.
Description
Technical Field
The invention belongs to the field of semiconductor photodetectors, and particularly relates to a TiN enhanced 4H-SiC-based broad spectrum photodetector with a vertical structure and a preparation method thereof.
Background
Photoelectric detectors based on conventional semiconductor materials such as silicon, germanium, group III arsenide, lead sulfide and the like are widely applied to the fields of optical fiber communication, laser ranging, industrial control, missile guidance, infrared sensing and the like. However, these photovoltaic devices made of conventional semiconductor materials cannot operate in extreme environments. Silicon carbide (SiC) is a wide bandgap semiconductor material and has the advantages of stable physical and chemical properties, large internal bond energy, low intrinsic carrier concentration, high average ionization energy, high critical displacement energy, and the like. Compared with devices made of traditional semiconductor materials, the SiC-based device is more suitable for extreme environments such as high temperature, strong radiation, complex chemical composition and the like. Most of the reported SiC photodetectors are fabricated on 4H-SiC substrates because high crystal quality 4H-SiC substrates have achieved wafer-level mass production. Unfortunately, due to the band gap limitations, 4H-SiC photodetectors are not responsive to visible or near infrared light where the photon energy is greater than its band gap, which limits their application to some extent. 2021, cui Yanxia et al disclose a patent (publication No. CN 113013278A) entitled "a silicon carbide-based full spectrum response photodetector and a method for producing the same", which realizes full spectrum detection of the photodetector by hot carrier principle by introducing a nanoparticle structure composed of gold, silver, titanium, nickel, palladium or cadmium into a metal-semiconductor-metal type 4H-SiC photodetector having a horizontal structure. However, the two functional electrodes of the 4H-SiC-based broad-spectrum response photodetector with the horizontal structure are fabricated on the same plane, have poor compatibility with a readout circuit, have weak environmental resistance, have poor stability in extreme environments, and do not match the extreme environmental resistance of SiC, and thus cannot be widely used.
Disclosure of Invention
The invention overcomes the defects existing in the prior art, and solves the technical problems that: a vertical structure TiN enhanced 4H-SiC-based broad spectrum photoelectric detector and a preparation method thereof are provided, so that the extreme environment tolerance of the photoelectric detector and the compatibility of the photoelectric detector with a read-out circuit are improved.
In order to solve the technical problems, the invention adopts the following technical scheme: a vertical structure TiN-enhanced 4H-SiC-based broad spectrum photodetector comprising: a top electrode layer, a TiN-NCCs layer, a semiconductor layer and Al which are sequentially arranged from top to bottom 2 O 3 The top electrode layer is a semitransparent metal electrode, the TiN-NCCs layer is TiN nano bulges formed by TiN materials and are formed by periodic arrangement on the surface of the semiconductor layer, the semiconductor layer is a 4H-SiC substrate, and the bottom electrode layer is an opaque metal electrode.
In the TiN-NCCs layer, the height of the highest part is 40nm plus or minus 5nm, the height of the lowest part is 0-20nm, the interval between adjacent TiN nano projections in the TiN-NCCs layer is 100nm plus or minus 10nm, and the duty ratio of the TiN nano projections in the structure is 80% plusor minus 10%.
The top electrode layer is TiN, and the bottom electrode material is Al.
The thickness of the semiconductor layer is 100-1000 mu m, the thickness of the top electrode layer is 15nm plus or minus 5nm, and the thickness of the bottom electrode layer is 100nm plus or minus 20nm.
The 4H-SiC substrate is semi-insulating, and the resistivity of the substrate is 1e13ohm cm-1 e15ohm cm.
The Al is 2 O 3 The thickness of the layer was 0.6 nm.+ -. 0.06nm.
In addition, the invention also provides a preparation method of the TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with the vertical structure, which comprises the following steps:
s1, cleaning a 4H-SiC substrate;
s2, using a PS nanosphere self-assembly method, and using PS nanosphere suspension to manufacture a PS nanosphere single-layer drainage layer on one surface of a 4H-SiC substrate, wherein the PS nanospheres are in a hexagonal close-packed structure with centers on one surface of the 4H-SiC substrate; then, etching the PS nanosphere single-layer arrangement layer by utilizing a reactive ion etching method to obtain an arranged PS nanosphere array;
s3, manufacturing a TiN film layer on one surface of the 4H-SiC substrate on which the PS nanosphere array is arranged by utilizing a magnetron sputtering method; then put it into toluene solution, make PS nanosphere array and TiN film layer above the array on the 4H-SiC base erode, get TiN-NCCs layer;
s4, continuously manufacturing a top electrode above the TiN-NCCs layer by utilizing a magnetron sputtering method;
s5, turning over the sample on the basis of the device with the top electrode manufactured by utilizing an atomic layer deposition method, and manufacturing Al on the other side of the 4H-SiC substrate 2 O 3 A layer;
s6, using a magnetron sputtering method to make Al 2 O 3 The layer shows that the bottom electrode is further fabricated.
In the step S2, the diameter of the PS nanospheres in the adopted PS nanosphere suspension is 100nm, methanol is adopted as a solvent, and the concentration is 2.5wt%.
In the step S2, in the PS nanosphere suspension, the diameter of the PS nanospheres is 100nm, methanol is used as a solvent, the concentration is 2.5wt%, and the diameter of the PS nanosphere array obtained after etching is 80+/-10 nm.
In the step S3, the 4H-SiC substrate after the TiN film layer is manufactured is put into toluene solution, after ultrasonic cleaning is performed for more than 30min, a sample is taken out, the surface of the sample is obtained by drying with nitrogen, and the sample is put into a culture dish for standby.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a vertical structure TiN enhanced 4H-SiC-based broad spectrum photoelectric detector and a preparation method thereof, wherein a top electrode and a bottom electrode are respectively arranged at two sides of a 4H-SiC semiconductor layer, and because two functional electrodes of the detector are distributed at two sides of the 4H-SiC, the detector has higher compatibility with a flip-chip bonding process of a read-out circuit, and the development of a low-cost area array imaging device is easier to realize. In addition, when the vertical structure device is manufactured, different materials and different processes can be selected for the top electrode and the bottom electrode, so that the device is beneficial to obtaining more excellent detection performance. In addition, when the vertical structure design is adopted, the distance between the electrodes can be finely adjusted, which is beneficial to regulating and controlling the optical resonance characteristic of the electrodes and realizing the optimization of the performance of the device.
2. The invention leads the bright current of the device in a wide spectrum range to be obviously improved by introducing a TiN nano-bulge structure (TiN-NCCs) at the interface of the 4H-SiC semiconductor layer and the top electrode layer, and in addition, leads 0.6nm Al at the interface of the 4H-SiC semiconductor layer and the bottom electrode layer 2 O 3 The layer acts as a modifier layer to suppress the rise in dark current of the device due to the introduction of TiN-NCCs. The vertical structure photoelectric detector without any addition is used as a contrast device, and a TiN-NCCs layer and Al are added at the same time 2 O 3 The devices of the layer have nearly the same dark current as the control devices. The TiN-NCCs have wide spectrum light absorption capacity in the wave band range of 400nm-1100nm, so that the high-efficiency generation of hot carriers is realized in an auxiliary manner. At 660nm wavelength, the bright current of the invention is 5.79nA, and the bright-dark current ratio is 1.7X10 4 The bright-dark current ratio is improved by about 82 times compared with the control device. At 1550nm wavelength, the bright current of the invention is 5.5pA, the bright-dark current ratio is 16, and compared with a control device, the bright-dark current ratio is improved by about 6 times. The TiN-NCCs layer is prepared by assistance of a low-cost Polystyrene (PS) nanosphere array template, and is prepared by taking etched PS nanospheres as templates and combining magnetron sputtering with a wet etching process. Therefore, the invention can realize TiN enhanced 4H-SiC base widthThe spectral photoelectric detector improves the bright-dark current specific performance of the device-near infrared wide spectral range.
Drawings
Fig. 1 is a schematic structural diagram of a vertical-structure TiN-enhanced 4H-SiC-based broad spectrum photodetector according to an embodiment of the present invention, where: 1-4H-SiC layer, 2-TiN-NCCs layer, 3-top electrode layer, 4-Al 2 O 3 Layer, 5-bottom electrode layer.
FIG. 2 is a schematic view (a) of PS nanospheres 6 used for preparing TiN-NCCs layers, AFM surface topography (b) of the prepared TiN-NCCs layers, and local AFM surface topography (c) of the TiN-NCCs layers in the examples of the present invention.
Fig. 3 is a graph showing the comparison of light absorption spectra of a substrate of a vertical-structure TiN-enhanced 4H-SiC-based broad-spectrum photodetector provided by an embodiment of the present invention before and after TiN-NCCs are introduced.
Fig. 4 is a graph showing current-voltage characteristics of a vertical-structure TiN-enhanced 4H-SiC-based broad spectrum photodetector in a dark state, and dark-state current-voltage characteristics of two control devices (TiN/4H-SiC/Al and TiN/TiN-NCCs/4H-SiC/Al) according to an embodiment of the present invention. Wherein when TiN is connected with positive and Al is connected with negative, the bias voltage V is applied a Greater than 0.
Fig. 5 is a graph showing the contrast of bright current of a vertical TiN-enhanced 4H-SiC-based broad spectrum photodetector and a control device (TiN/4H-SiC/Al) under the irradiation of incident light with different wavelengths (λ), where λ=660 nm, 850nm, 980nm, 1310nm and 1550nm, the light power received by the effective area region of the device is 0.4mW, and the bias voltage is 20V.
Fig. 6 is a graph showing the contrast of light and dark current of a TiN-enhanced 4H-SiC-based broad spectrum photodetector with a vertical structure and a control device (TiN/4H-SiC/Al) under the irradiation of incident light with different wavelengths (λ), where λ=660 nm, 850nm, 980nm, 1310nm and 1550nm, the light power received by the effective area region of the device is 0.4mW, and the applied bias voltage is 20V.
FIG. 7 is a graph showing the current-voltage characteristics of a vertical TiN-enhanced 4H-SiC-based broad spectrum photodetector and a control device (TiN/4H-SiC/Al) according to an embodiment of the present invention when the wavelength of incident light is 660nm (the optical power is 0.4 mW).
FIG. 8 is a graph showing transient current characteristics of a vertical TiN enhanced 4H-SiC-based broad spectrum photodetector with 660nm wavelength under 5V bias conditions.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in FIG. 1, the first embodiment of the invention provides a vertical-structure TiN enhanced 4H-SiC-based broad spectrum photodetector, which comprises a top electrode layer 3, a TiN-NCCs layer 2, a semiconductor layer 1 and Al which are sequentially arranged from top to bottom 2 O 3 The top electrode layer 3 is a semitransparent metal electrode, the TiN-NCCs layer 2 is TiN nano bulges formed by TiN materials and are formed by periodic arrangement on the surface of the semiconductor layer 1, the semiconductor layer 1 is a 4H-SiC substrate, and the bottom electrode layer 5 is an opaque metal electrode.
Specifically, as shown in fig. 2 (a), in this example, a schematic diagram of a PS nanosphere array template for preparing the TiN-NCCs layer 2 was shown. The PS nanosphere structure is prepared by firstly preparing a PS nanosphere array structure with the diameter of 100nm on a 4H-SiC semiconductor layer, wherein the PS nanosphere array is in a short-range ordered periodic central filled hexagonal close-packed structure, and then the PS nanospheres are etched to reduce the diameter to 80+/-5 nm, namely the PS nanospheres 6 shown in fig. 2 (a). Then, a layer of TiN material with the thickness of 40nm plus or minus 5nm is magnetically sputtered on the surface of the PS nanospheres 6, so that the TiN material is distributed in the etched PS nanospheres, finally, the PS nanospheres and the TiN material on the upper layer of the PS nanospheres are washed away, and due to the shielding shadow effect of the PS nanospheres during preparation, the TiN-NCCs layer formed by periodically hexagonal close-packed TiN nanospheres is finally obtained, wherein the AFM morphology is as shown in fig. 2 (b), and the interval between adjacent nanospheres is 100nm plus or minus 10nm. FIG. 2 (c) shows an AFM partial enlargement of a region of a TiN-NCCs layer. The relative heights of the TiN nano bumps shown in FIG. 2 (c) are about 10-20nm, and since the total thickness of the TiN film is 40nm, the heights of the highest and lowest positions of the nano TiN bumps in FIG. 2 (c) can be calculated to be 40nm and 20-30 nm, respectively. In addition, since the shadow effect of PS nanospheres is most severe just below their center, the TiN material is plated in this region to a minimum thickness, approximately between 0-10 nm.
Specifically, in this embodiment, the height of the highest portion of the raised region in the TiN-NCCs layer is 40nm±5nm, and furthermore, in the TiN-NCCs layer, the height of the lowest portion of the center of the region covered with PS nanospheres is 0 to 20nm, i.e., the height of the highest portion in the TiN-NCCs layer is 40nm±5nm, the height of the lowest portion is 0 to 20nm, the interval between adjacent TiN nanobumps in the TiN-NCCs is 100nm±10nm, and the duty ratio of the TiN nanobumps in the structure is 80% ±10%.
Preferably, in this embodiment, the height of the highest part in the TiN-NCCs layer is 40nm±5nm, the height of the lowest part is 0 to 20nm, the interval between adjacent TiN nano-protrusions in the TiN-NCCs layer is 100nm±2nm, and the duty ratio of the TiN nano-protrusions in the structure is 80% ±2%.
Further, in this embodiment, the top electrode layer is TiN, and the bottom electrode material is Al. The whole structure of the device is TiN/TiN-NCCs/4H-SiC/Al 2 O 3 /Al。
Further, in this embodiment, the thickness of the semiconductor layer is 100 to 1000 μm, the thickness of the top electrode layer is 15 nm.+ -. 5nm, and the thickness of the bottom electrode is 100 nm.+ -. 20nm.
Further, in this example, the 4H-SiC substrate was semi-insulating, and the resistivity thereof was 1e13 ohm-cm to 1e15 ohm-cm.
Further, in the present embodiment, the Al 2 O 3 The thickness of the layer was 0.6 nm.+ -. 0.06nm. Preferably, in the present embodiment, the Al 2 O 3 The thickness of the layer was 0.6nm.
The embodiment of the invention provides a TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with a vertical structure, which comprisesThe embodiment of the invention enhances the wide-spectrum photocurrent by introducing TiN-NCCs into an ultraviolet photoelectric detector formed by a top electrode, a semiconductor layer and a bottom electrode, and simultaneously introduces Al 2 O 3 The layer is used as an interface modification layer to inhibit the dark current degradation of the device caused by the introduction of TiN-NCCs, and improves the weak light detection performance of the ultraviolet photoelectric detector. At 660nm wavelength (0.4 mW power), the bright current of the invention is 5.7nA, and the bright-dark current ratio is 1.7X10 4 The method comprises the steps of carrying out a first treatment on the surface of the In contrast, under the same test conditions, tiN-NCCs and Al are not added 2 O 3 The control device of the layer had a 60pA bright current and 2.0X10 2 Is a ratio of light to dark current. At 1550nm wavelength, the bright current of the invention is 4.6pA, and the bright-dark current ratio is 16; in contrast, under the same test conditions, tiN-NCCs and Al are not added 2 O 3 The control device of the layer had a bright current of 0.8pA and a bright-dark current ratio of 2.6.
Example two
The second embodiment of the invention provides a preparation method of a TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with a vertical structure, wherein the adopted materials are as follows:
4H-SiC substrate, tiN target material, al target material, hydrogen peroxide, ammonia water, deionized water, sulfuric acid, nitric acid, detergent, deionized water, acetone, absolute ethyl alcohol, trimethylaluminum, ps nanosphere suspension (2.5 wt% aqueous solution), methanol and metal mask. The combined dosage and the screening standard are as follows:
4H-SiC substrate: semi-insulating, weak n-type, resistivity of 1e14 ohm cm, area of 20mm×20mm, thickness of 500 μm;
TiN target: binding a solid, copper back plate, 99.9% purity;
al target: binding a solid, copper backboard, and 99.999% purity;
hydrogen peroxide: h 2 O 2 ，3％；
Ammonia water: NH (NH) 4 OH:H 2 O，25％
Deionized water: h 2 O 8000mL±50mL；
Sulfuric acid: h 2 SO 4 ，98％
Nitric acid：HNO 3 ，68％
Liquid detergent: 2+ -0.5 mL;
acetone: CH (CH) 3 COCH 3 250 mL±5mL；
Absolute ethyl alcohol: c (C) 2 H 5 OH 500mL±5mL；
Toluene: c (C) 7 H 8 500mL±5mL；
Methanol: CH (CH) 3 OH 500mL±5mL；
Trimethylaluminum: c (C) 3 H 9 100mL + -5 mL of Al 1.0M hexane solution;
PS nanosphere suspension: methanol with the diameter of 100nm is used as a solvent, and the concentration is 2.5 weight percent;
metal mask plate: stainless steel; and (3) bar-shaped patterns, wherein the hollowed-out width is 2mm, and the spacing is 5mm.
The preparation method of the TiN enhanced 4H-SiC-based broad spectrum photoelectric detector with the vertical structure provided by the embodiment specifically comprises the following steps:
s1, cleaning the 4H-SiC substrate.
In the step S1, the method for cleaning the 4H-SiC substrate comprises the following steps:
s101, using a measuring cylinder to mix hydrogen peroxide, ammonia water and deionized water into a mixture according to a ratio of 10:10:1, then placing a 4H-SiC substrate into a solution, covering the mouth of the beaker by aluminum foil paper, soaking for more than 20 minutes, then taking out the 4H-SiC substrate, flushing with clear water, and removing residual solution;
s102, adding deionized water into another polytetrafluoroethylene beaker to obtain a solution of 4:1, putting a 4H-SiC substrate into the nitric acid solution with diluted proportion, covering a beaker opening by aluminum foil paper, performing ultrasonic treatment for 30min, taking out the 4H-SiC substrate, flushing with clear water, and removing residual solution;
s103, coating detergent on the surface of the sheet, repeatedly rubbing and cleaning the 4H-SiC substrate under water flow until the surface of the 4H-SiC substrate can form an aggregated water film when the cleaning is performed by using clear water.
S104, then, vertically placing the 4H-SiC substrate on a beaker holder, placing the beaker holder in a glass beaker, sequentially adding deionized water and acetone, and respectively carrying out ultrasonic treatment on the absolute ethyl alcohol solution for 15min. To this end, the 4H-SiC substrate was cleaned, and the cleaned 4H-SiC substrate was placed in a beaker containing an isopropyl alcohol solution for use.
S2, using a PS nanosphere self-assembly method, and using PS nanosphere suspension to manufacture a PS nanosphere single-layer drainage layer on one surface of a 4H-SiC substrate, wherein the PS nanospheres are in a hexagonal close-packed structure with centers on one surface of the 4H-SiC substrate; and then, etching the PS nanosphere monolayer arrangement layer by utilizing a reactive ion etching method to obtain the arranged PS nanosphere array.
In the step S2, the diameter of the PS nanospheres in the adopted PS nanosphere suspension is 100nm, methanol is adopted as a solvent, and the concentration is 2.5wt%.
Specifically, in the step S2, in the PS nanosphere suspension, the diameter of the PS nanosphere is 100nm, methanol is used as a solvent, the concentration is 2.5wt%, and the diameter of the PS nanosphere obtained after the etching is completed is 80±10nm.
Specifically, in this embodiment, the step S2 specifically includes the following steps:
s201, adding hydrogen peroxide, ammonia water and deionized water into a glass beaker according to the ratio of 10:10:1 by using a measuring cylinder, then drying the cleaned 4H-SiC substrate by using nitrogen, putting the dried 4H-SiC substrate into a solution, enabling the substrate to fully contact the solution by using a PS beaker frame, covering a beaker opening by using aluminum foil paper, soaking for 10min, and then taking out the 4H-SiC substrate;
s202, adding concentrated sulfuric acid and hydrogen peroxide into a glass beaker according to the ratio of 4:1 by using a measuring cylinder, then placing the 4H-SiC substrate treated by the S201 into the prepared solution, enabling the substrate to fully contact with the solution by using a PS beaker frame, covering a cup mouth by using aluminum foil paper, soaking for 20min, then taking out the 4H-SiC substrate, flushing by using deionized water, removing surface residual solution, and placing into deionized water for standby;
s203, adding PS nanosphere suspension (100 nm diameter, 2.5wt% aqueous solution) and methanol solution into a glass bottle in a ratio of 1:2 by using a syringe, and performing ultrasonic treatment at normal temperature for 5min;
s204, drying the 4H-SiC substrate subjected to surface treatment by using nitrogen, placing the substrate on a reverse-buckling culture dish, and dripping a proper amount of deionized water on the substrate;
s205, extracting an appropriate amount of solution from a glass bottle by using an injector, fixing the injector on the pump injector, adjusting the height of the pump injector to ensure that the injection head of the injector is equal to the height of the 4H-SiC substrate, setting the injection rate of the pump to be 0.5mL/min, slowly injecting the prepared PS suspension onto the substrate from one corner of the substrate, observing that the PS nanospheres are self-assembled into a single-layer film on opposite corners due to the pushing of a tension water film to opposite corners by naked eyes, and continuously expanding the assembled PS nanosphere array towards the corners of the injector along with the increase of the injected suspension until finally adjusting the injection rate of the pump to be 0.25mL/min, so that the quantity of the injected suspension is reduced to ensure that the single-layer arrangement area of the PS nanospheres is as large as possible;
s206, after the whole water film is basically covered by the single-layer PS nanosphere array, placing a reversely-buckled culture dish and a sample on a hot plate at 60 ℃ to heat the sample for about 2 hours at intervals, controlling volatilization and convection speeds, completely evaporating the water film, and leaving the PS nanosphere array densely distributed in two-dimensional hexagons on a 4H-SiC substrate;
s207, taking the 4H-SiC substrate with the PS nanosphere arrays arranged thereon off a hot table and placing the substrate into a culture dish for standby;
s208, opening a flowmeter and an oxygen flow switch of the reactive ion etching machine, adjusting the oxygen flow to a proper flow, opening a cabin door of the reactive ion etching machine, placing 4H-SiC with the PS nanosphere array arranged in the cabin door of the etching machine, closing the cabin door, and opening a vacuum pump.
S209, when the pressure in the cabin reaches 5pa, an etching power supply of the reactive ion etching machine is turned on, the etching power knob is adjusted to 30W, glow appears in the cabin, and etching is started. The etching process is continued for a certain time to reduce the size of the PS nanospheres to the desired size.
And S210, after the etching process is finished, adjusting the power to be in an off state, closing an etching power supply, closing a vacuum pump, opening a cabin door air release switch, opening the cabin door when the pressure in the cabin rises to the atmospheric pressure, and taking out the etched 4H-SiC substrate. And placing the 4H-SiC substrate loaded with the PS nanosphere array template in a culture dish for standby.
S3, manufacturing a TiN film layer on one surface of the 4H-SiC substrate on which the PS nanosphere array is arranged by utilizing a magnetron sputtering method; and then putting the substrate into toluene solution to enable the PS nanosphere array on the 4H-SiC substrate and the TiN film layer above the array to be corroded, thus obtaining the TiN-NCCs layer.
In the step S3, the 4H-SiC substrate after the TiN film layer is manufactured is put into toluene solution, after ultrasonic cleaning is performed for more than 30min, a sample is taken out, the surface of the sample is obtained by blowing nitrogen to dry, and the sample is put into a culture dish for standby.
Specifically, in this embodiment, the step S3 specifically includes the following steps:
s301, mounting a TiN target material to be sputtered on a radio frequency sputtering target head of a magnetron sputtering coating machine.
S302, loading one side of the 4H-SiC substrate loaded with the PS nanosphere array template downwards on a sample support of a magnetron sputtering coating machine, wherein the film growth surface at the moment is the side loaded with the PS nanosphere array template, and the surface is downwards, and adjusting the sample support to enable the 4H-SiC substrate to be positioned right above a target.
S303, closing a magnetron sputtering cabin door, opening a vacuum gauge, zeroing, opening a mechanical pump and a pre-pumping valve on a display screen, closing the pre-pumping valve when the pressure drops to 30Pa, and opening a gate valve and a molecular pump, wherein the cabin body pressure reaches 10 -4 And when the Pa magnitude is reached, opening an argon ionization valve and an argon channel power supply.
S304, sequentially opening an argon magnetic control valve, a mechanical valve and a flowmeter, selecting proper argon flow, and then adjusting a gate valve of a molecular pump to maintain the cavity pressure at 2Pa.
S306, turning on a sputtering power supply, adjusting the power required by sputtering, and further adjusting the pressure through a gate valve after starting so that the sputtering rate reaches the film forming requirement. Pre-sputtering for 10min, and then performing formal sputtering. When the required film thickness is reached, the large baffle is closed, then the sputtering power supply is closed, the sample is taken out from the film plating chamber, and the sample is put into a culture dish for standby.
S306, pouring a proper amount of toluene solution into a glass beaker, putting the 4H-SiC substrate loaded with the PS nanosphere array template and the TiN film into the solution, carrying out ultrasonic cleaning for 30min with the structure facing downwards, taking out a sample, drying with nitrogen to obtain the surface of the sample, and putting the sample into a culture dish for standby.
S4, continuously manufacturing a top electrode above the TiN-NCCs layer by utilizing a magnetron sputtering method.
In the step S4, the method for manufacturing the top electrode includes:
s401, mounting a TiN target material to be sputtered on a radio frequency sputtering target head of a magnetron sputtering coating machine.
And S402, attaching a metal mask plate on one side of the 4H-SiC substrate with the nano concave-convex structure, then loading the metal mask plate on a sample support of a magnetron sputtering coating machine, wherein the film growth surface is the surface on which the metal mask plate is loaded, and adjusting the sample support to enable the 4H-SiC substrate to be positioned right above the target.
S303, closing a magnetron sputtering cabin door, opening a vacuum gauge, zeroing, opening a mechanical pump and a pre-pumping valve on a display screen, closing the pre-pumping valve when the pressure drops to 30Pa, and opening a gate valve and a molecular pump, wherein the cabin body pressure reaches 10 -4 And when the Pa magnitude is reached, opening an argon ionization valve and an argon channel power supply.
S404, sequentially opening an argon magnetic control valve, a mechanical valve and a flowmeter, selecting proper argon flow, and then adjusting a gate valve of a molecular pump to maintain the cavity pressure at 2Pa.
S405, turning on a sputtering power supply, adjusting the power required by sputtering, and further adjusting the pressure through a gate valve after starting so that the sputtering rate reaches the film forming requirement. Pre-sputtering for 10min, and then performing formal sputtering. When the required film thickness is reached, the large baffle is closed, then the sputtering power supply is closed, the sample is taken out from the film plating chamber, and the metal mask is removed.
S5, turning over the sample on the basis of the device with the top electrode manufactured by utilizing an atomic layer deposition method, and manufacturing Al on the other side of the 4H-SiC substrate 2 O 3 A layer.
In the step S5, al 2 O 3 The manufacturing method of the layer comprises the following steps:
s501, turning over a sample plated with the semitransparent top electrode, attaching a metal mask plate on the other side of the 4H-SiC substrate for standby, and taking care of protecting the prepared film layer.
S502, opening circulating water for refrigeration, inflating to open a cabin door, tightly installing a trimethylaluminum and water vapor raw material bottle and a manual valve, closing the cabin door, setting the temperature of a deposition chamber to 150 ℃ through a computer, setting the flow of carrier gas to 30sccm after the temperature is stable, setting the type, time, flow, reaction time and cleaning time of each raw material, and controlling the deposition speed to be 0.06nm per cycle. The wait time was set to 1 minute and the pre-deposition 40 cycle was started.
And S503, after the pre-deposition is finished, inflating and opening the cabin door, loading the sample loaded with the metal mask plate into the atomic layer deposition chamber, ensuring that the growth surface of the film faces upwards, starting formal deposition, and setting proper circulation times to meet the required film thickness requirement.
And S504, when the film thickness requirement is met, the deposition is automatically completed, when the temperature of the deposition chamber is reduced to the room temperature, the sample is taken out through inflation, the metal mask is not removed, and the next step is prepared. And then, vacuumizing the instrument, closing the manual valve, and evacuating all residual raw materials in the pipeline. And (3) inflating the air to the atmospheric pressure, closing the vacuum pump, stopping heating, and closing the power switch of the equipment when the temperature is reduced to the room temperature.
S6, using a magnetron sputtering method to make Al 2 O 3 The layer shows that the bottom electrode is further fabricated.
In the step S6, the manufacturing method of the bottom electrode includes:
s601, mounting an Al target to be sputtered on a direct current sputtering target head of a magnetron sputtering coating machine.
S602, loading the 4H-SiC substrate with the well-grown interface modification layer on a sample support of a magnetron sputtering coating machine, wherein the growth surface of the film is added with Al 2 O 3 One side of the interface modification layer, facing down, was adjusted to position the 4H-SiC substrate directly over the target.
S603, closing the magnetron sputtering cabin door, opening and zeroing the vacuum gauge, opening the mechanical pump and the pre-pumping valve on the display screen, closing the pre-pumping valve when the pressure drops to 30Pa, and opening the plug-in valvePlate valve and molecular pump with cabin pressure up to 10 -4 And when the Pa magnitude is reached, opening an argon ionization valve and an argon channel power supply.
S604, sequentially opening an argon magnetic control valve, a mechanical valve and a flowmeter, selecting proper argon flow, and then adjusting a gate valve of a molecular pump to maintain the cavity pressure at 2Pa.
S605, a direct-current sputtering power supply is turned on, the power required by sputtering is regulated, after starting, the pressure is further regulated through a gate valve, the sputtering rate reaches the film forming requirement, and sputtering is performed for 10 minutes. And finally, performing formal sputtering, namely closing the large baffle plate and then closing the sputtering power supply until the required film thickness is reached, taking out a sample from the film coating chamber, removing the metal mask plate, and collecting the sample.
Detection, analysis and characterization: and detecting, analyzing and characterizing the performance of the prepared 4H-SiC electrical detector.
Measuring a current-voltage characteristic curve of the device in a dark state by using a high-precision digital source meter AglientB 1500; the current-voltage characteristic curve and the transient photocurrent response curve of the 4H-SiC broad spectrum photoelectric detector in a bright state are measured by AglientB1500 by using Thorolabs 660nm, 850nm LEDs and 980nm, 1310nm and 1550nm lasers of vincristal industries as light sources. And testing the transmission spectrum and the reflection spectrum of the substrate before and after the TiN-NCCs by using a multiplexing integrating sphere spectrum test system, and converting to obtain the absorption spectrum of each sample.
Conclusion: analysis of vertical TiN/TiN-NCCs/4H-SiC Al with TiN nano concave-convex structure and interface modification layer 2 O 3 Dark state current-voltage characteristic curves of/Al broad spectrum photodetectors and control devices (TiN/4H-SiC/Al, tiN/TiN-NCCs/4H-SiC/Al) and bright state current-voltage characteristic curves at the 4H-SiC non-light absorption band.
Fig. 3 shows a comparison of the optical absorption spectra of a 4H-SiC substrate layer of a photodetector of the present invention before and after the introduction of TiN-NCCs. The TiN-NCCs layer has wide spectrum light absorption capacity in the wave band range of 400nm-1100nm, and the high-efficiency generation of hot carriers is realized in an auxiliary manner.
FIG. 4 shows a vertical structure of TiN/TiN-NCCs/4H-SiC/Al with TiN nano relief structure and interface modification layer 2 O 3 Dark state current-voltage characteristic curves of the Al broad spectrum photodetector and the control device (TiN/4H-SiC/Al). The dark current of the device is subject to synergy of three mechanisms: 1) The semi-insulating 4H-SiC substrate layer has low intrinsic carrier concentration, and accordingly, dark current caused by the intrinsic carrier is low; 2) The energy level of the semi-insulating 4H-SiC basal layer is the Fermi energy level clamped by a surface state, the height of a potential barrier formed after metal is contacted with the metal is irrelevant to the work function of the metal, the potential barrier during carrier injection is far higher than the energy of a thermally excited carrier, and accordingly, the injection current is effectively inhibited; 3) Introduction of Al 2 O 3 And the layer modifies the surface state of the 4H-SiC substrate, and accordingly, dark current caused by interface charge is effectively inhibited. The three mechanisms work together, so that the addition of TiN-NCCs cannot influence the dark state performance of the device. Lack of Al 2 O 3 The dark state current of the circuit control device TiN/4H-SiC/Al of the layer at 20V bias voltage is 3.1X10 -13 A, and the dark current after adding TiN-NCCs layer is changed to 3.4X10 only -13 A, namely the TiN-NCCs layer has negligible effect on the dark current of the detector. And when Al is not present 2 O 3 When the interface is modified, the dark state current of the reference control device TiN/TiN-NCCs/4H-SiC/Al under the bias voltage of 20V is 3.0x10 -11 The dark state performance of the device is attenuated sharply, and changes of nearly two orders of magnitude occur.
FIG. 5 shows a vertical structure of TiN/TiN-NCCs/4H-SiC/Al according to an embodiment of the invention 2 O 3 A histogram of bright current of the device as a function of wavelength when the incident light is light in the 4H-SiC non-light absorption band at 20V bias voltage for a/Al broad spectrum photodetector and a control device (TiN/4H-SiC/Al). As can be seen from the graph, after the TiN nano concave-convex structure is added, the bright state current of the device is higher than that of the control device in the non-light absorption wave band of 4H-SiC, and the bright state current is 6.29 multiplied by 10 when the irradiation wavelength is 660nm -11 A is lifted to 5.79 multiplied by 10 -9 A, the lifting is about 89 times; at 850nm from 5.54×10 -11 A is lifted to 2.13 multiplied by 10 - 10 A, 3 times of improvement; at 980nm from 5.10X10 -12 A is promoted to 3.04 multiplied by 10 -11 A, the lifting is 5 times; 1310nm from 6.49×10 -12 A is lifted to 5.81×10 -11 A, 8 times of improvement; at 1550nm from 8.05X10 -13 A is lifted to 5.5X10 -12 A, the lifting is about 5 times. And due to the synergistic effect of multiple dark current inhibition mechanisms, the bright-dark current ratio is also enhanced by the addition of the TiN nano concave-convex structure.
FIG. 6 shows a vertical structure of TiN/TiN-NCCs/4H-SiC/Al according to an embodiment of the invention 2 O 3 A histogram of the ratio of bright to dark current of the device as a function of wavelength when the incident light is light in the 4H-SiC non-light absorption band at a bias voltage of 20V for a broad spectrum photo detector of/Al and a control device (TiN/4H-SiC/Al), the ratio of bright to dark current being increased from 205 to 1.7X10 when the irradiation wavelength is 660nm 4 About 82 times higher; at 850nm, the wavelength is increased from 180 to 626, and is increased by 2.5 times; lifting from 16 to 89 at 980nm, 4.5 times; at 1310nm, the wavelength is increased from 21 to 171, 8 times; lifting from 2.6 to 16 at 1550nm, 6-fold improvement.
In a word, the wide spectrum detector of the invention can greatly improve the bright current of the device in the 660nm, 850nm, 980nm, 1310nm and 1550nm wave bands which are not absorbed by 4H-SiC through the TiN-NCCs layer with nanometer concavo-convex shape on the basis of basically maintaining dark current. Because 4H-SiC is a wide band gap semiconductor, the visible and near infrared bands are weak correspondingly, and TiN is used as a transition metal nitride which has a plurality of similar physical properties with Au, and when the transition metal nitride is used for replacing Au, the cost can be greatly reduced, and simultaneously, better photoelectric performance is realized by utilizing the wider absorption spectrum relative to Au. The energy level of the semi-insulating 4H-SiC is the Fermi energy level clamped by the surface state, so that hot carriers can cross potential barriers more easily, the response spectrum of the device is further widened, and the bright state response is more excellent.
FIG. 7 shows a vertical structure of TiN/TiN-NCCs/4H-SiC/Al according to an embodiment of the invention 2 O 3 A bright state current-voltage characteristic curve of the Al broad spectrum photodetector and the control device (TiN/4H-SiC/Al) with the incident light of 660nm and the optical power of 0.4 mW. As can be seen from fig. 7, the bright current of the present invention is higher than that of the control device at different voltages. FIG. 8 shows a vertical structure of TiN/TiN-NCCs/4H-SiC/Al with TiN nano relief structure and interface modification layer 2 O 3 The transient current characteristic curve of the Al broad spectrum photoelectric detector under the incident light of 660nm and the bias voltage of 5V can be seen from the graph, and the invention can give stable current response under the incident light pulse condition.
In summary, the invention provides a vertical structure broad spectrum photoelectric detector based on a semi-insulating 4H-SiC substrate and a preparation method thereof, and the invention is based on a metal electrode-4H-SiC-metal electrode structure of a vertical structure, and by introducing an atomically thick modification layer at the interface of the 4H-SiC and a bottom electrode and introducing a TiN nano concave-convex structure at the interface of the 4H-SiC and a top electrode, the response spectrum of the device is effectively widened, so that the detectable wavelength of the device is widened to 1550nm.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. A vertical structure TiN-enhanced 4H-SiC-based broad spectrum photodetector, comprising: a top electrode layer, a TiN-NCCs layer, a semiconductor layer and Al which are sequentially arranged from top to bottom 2 O 3 The top electrode layer is a semitransparent metal electrode, the TiN-NCCs layer is TiN nano bulges formed by TiN materials and are formed by periodic arrangement on the surface of the semiconductor layer, the semiconductor layer is a 4H-SiC substrate, and the bottom electrode layer is an opaque metal electrode; in the TiN-NCCs layer, the highest height is 40nm +/-5 nm, the lowest height is 0-20nm, the interval between adjacent TiN nano bumps in the TiN-NCCs layer is 100nm +/-10 nm, and the duty ratio of the TiN nano bumps in the structure is 80% +/-10%.
2. The vertical structure TiN enhanced 4H-SiC based broad spectrum photodetector of claim 1, wherein said top electrode layer is TiN and said bottom electrode material is Al.
3. The vertical-structure TiN-enhanced 4H-SiC-based broad spectrum photodetector according to claim 1, wherein the thickness of the semiconductor layer is 100-1000 μm, the thickness of the top electrode layer is 15nm ±5nm, and the thickness of the bottom electrode is 100nm ±20nm.
4. The vertical structure TiN enhanced 4H-SiC-based broad spectrum photodetector of claim 1, wherein the 4H-SiC substrate is semi-insulating with a resistivity of 1e13ohm cm to 1e15ohm cm.
5. The vertical structure TiN enhanced 4H-SiC-based broad spectrum photodetector of claim 1, wherein said Al 2 O 3 The thickness of the layer was 0.6 nm.+ -. 0.06nm.
6. The method for manufacturing the vertical-structure TiN-enhanced 4H-SiC-based broad-spectrum photoelectric detector according to any one of claims 1 to 5, which is characterized by comprising the following steps:
s1, cleaning a 4H-SiC substrate;
s2, using a PS nanosphere self-assembly method, and using PS nanosphere suspension to manufacture a PS nanosphere single-layer drainage layer on one surface of a 4H-SiC substrate, wherein the PS nanospheres are in a hexagonal close-packed structure with centers on one surface of the 4H-SiC substrate; then, etching the PS nanosphere single-layer arrangement layer by utilizing a reactive ion etching method to obtain an arranged PS nanosphere array;
s3, manufacturing a TiN film layer on one surface of the 4H-SiC substrate on which the PS nanosphere array is arranged by utilizing a magnetron sputtering method; then put it into toluene solution, make PS nanosphere array and TiN film layer above the array on the 4H-SiC base erode, get TiN-NCCs layer;
s4, continuously manufacturing a top electrode above the TiN-NCCs layer by utilizing a magnetron sputtering method;
s5, utilizingAtomic layer deposition method, on the basis of the device with top electrode, turning over the sample, and making Al on the other side of 4H-SiC substrate 2 O 3 A layer;
s6, using a magnetron sputtering method to make Al 2 O 3 The layer shows that the bottom electrode is further fabricated.
7. The method for preparing the vertical-structure TiN enhanced 4H-SiC-based broad spectrum photoelectric detector according to claim 6, wherein in the step S2, the diameter of the PS nanospheres in the adopted PS nanosphere suspension is 100nm, methanol is adopted as a solvent, and the concentration is 2.5wt%.
8. The method for preparing a vertical-structure TiN-enhanced 4H-SiC-based broad spectrum photodetector according to claim 6, wherein in said step S2, PS nanospheres are 100nm in diameter in PS nanosphere suspension, methanol is used as solvent, the concentration is 2.5wt%, and the diameter of PS nanosphere array obtained after etching is 80±10nm.
9. The method for preparing a vertical structure TiN enhanced 4H-SiC-based broad spectrum photodetector according to claim 6, wherein in step S3, the 4H-SiC substrate after the TiN thin film layer is prepared is put into toluene solution, and after ultrasonic cleaning for more than 30min, the sample is taken out, and the surface of the sample is obtained by drying with nitrogen gas and put into a culture dish for standby.
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