CN114823945B - Detector structure of metal/titanium doped tungsten oxide Schottky junction and preparation method - Google Patents

Detector structure of metal/titanium doped tungsten oxide Schottky junction and preparation method Download PDF

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CN114823945B
CN114823945B CN202210450327.3A CN202210450327A CN114823945B CN 114823945 B CN114823945 B CN 114823945B CN 202210450327 A CN202210450327 A CN 202210450327A CN 114823945 B CN114823945 B CN 114823945B
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tungsten oxide
doped tungsten
titanium
metal
titanium doped
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张响
王晓强
林必堉
孙志华
申富升
吕航
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Northeastern University Qinhuangdao Branch
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Abstract

The invention discloses a detector structure of a metal/titanium doped tungsten oxide Schottky junction and a preparation method thereof, and relates to the field of photoelectric detector manufacturing. Specifically, fluorine-doped tin oxide (FTO) conductive glass is used as a substrate; depositing a titanium doped tungsten oxide layer on one side surface of the FTO conductive glass substrate by utilizing a magnetron sputtering method; placing the material into a muffle furnace for high-temperature heat treatment, and crystallizing tungsten oxide to enable the surface to generate an inward sinking structure; and depositing metal on the surface of the FTO conductive glass with the titanium doped tungsten oxide layer after heat treatment by utilizing a magnetron sputtering or vacuum evaporation method. The invagination structure enables the metal surface of the final device to have a plasmon effect so as to enhance the absorption and conversion efficiency of the device to incident light and realize the widening of response spectrum, breaks through the limit of the forbidden bandwidth of the traditional inorganic material detector, and further obtains the high-performance wide-spectrum photoelectric detector.

Description

Detector structure of metal/titanium doped tungsten oxide Schottky junction and preparation method
Technical field:
the invention belongs to the technical field of manufacturing of hot electron photoelectric detectors, and particularly relates to a detector structure of a metal/titanium doped tungsten oxide Schottky junction and a preparation method thereof, which are particularly used for photoelectric detection.
The background technology is as follows:
the photoelectric detector can convert optical signals into electric signals and has very wide application in the fields of optical communication, temperature measurement, imaging and the like. The inorganic photoelectric detector has the advantages of rich raw materials, easy acquisition, high carrier mobility and the like. However, the conventional inorganic semiconductor has a limited application range because it can only detect light waves having energy higher than the forbidden bandwidth. In recent years, thermionic photoelectric conversion based on surface plasmon induction has been favored. The surface plasmon induced thermal electrons can be rapidly transferred and realize high-efficiency photoelectric conversion, because the transfer speed of the thermal electrons is less than 100 femtoseconds, the energy loss and the corresponding prolonged response time caused by the competition of the thermal electrons and the processes of relaxation, recombination, binding and the like of carriers are avoided; also, in the case where the wavelength of the incident light is smaller than the semiconductor band gap width, plasmon-induced hot electrons can still be excited from the vicinity of the fermi surface to a higher energy level, generating photocurrent, i.e., surface plasmon-based photodetection is in principle not limited by the semiconductor band.
Schottky junctions are commonly used to fabricate various devices such as microwave diodes, avalanche diodes, and photodiodes. Schottky junctions are interfaces composed of metal and semiconductor, and have nonlinear impedance characteristics similar to the PN junctions of semiconductors. The band of the semiconductor at the interface of the schottky junction is bent to form a potential barrier, and only electrons having energies higher than the potential barrier may cross the potential barrier.
The invention comprises the following steps:
the invention aims to overcome the defects in the prior art and provide a detector structure of a metal/titanium doped tungsten oxide Schottky junction and a preparation method thereof, and the detector structure is particularly used for photoelectric detection and is based on the Schottky junction.
The Schottky junction has an internal photoelectric effect, is simple to prepare and has a high light response speed; the device embryonic form is generated by adopting a magnetron sputtering method with high yield, and the device can stably enhance the absorption efficiency of incident light under the conditions of low cost and easy preparation of the device. Meanwhile, the tungsten oxide is crystallized and conformal through heat treatment, namely, the surface of the tungsten oxide is provided with a shape with high and low fluctuation and larger specific surface area through heat treatment, so that the effective area of Schottky junction contact formed by the subsequently deposited metal and the tungsten oxide is obviously improved, and the surface plasmon effect is generated to widen the spectral range of the response of the device, thereby improving the performance of the device.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the detector structure of the metal/titanium doped tungsten oxide Schottky junction sequentially comprises an FTO glass layer, a titanium doped tungsten oxide layer with an invagination structure and a metal film layer from bottom to top, wherein the thickness of the FTO glass layer is 200nm, the thickness of the titanium doped tungsten oxide layer is 30-40 nm, the metal is gold or aluminum, and the thickness of the metal film layer is 20-30 nm.
The FTO glass layer is formed by attaching the FTO layer to one side of the glass substrate.
The titanium mass percentage of the titanium doped tungsten oxide layer is less than or equal to 5 percent.
The titanium mass percentage content in the titanium doped tungsten oxide layer is preferably 2.5-5%.
The preparation method of the detector structure of the metal/titanium doped tungsten oxide Schottky junction comprises the following steps:
step one, FTO glass layer treatment
Taking the FTO glass layer as a substrate, and performing secondary cleaning after primary cleaning and drying;
in the first step, the primary cleaning mode is that deionized water, absolute ethyl alcohol and acetone are sequentially used for ultrasonic cleaning in an ultrasonic cleaning machine for 10-15 min respectively; drying operation and constant temperature oven at 60-80deg.C, and cleaning in plasma cleaning machineThe line is cleaned for 6-8min; the sputtering mode is vacuum magnetron sputtering, and the pressure in the vacuum chamber of the magnetron sputtering needs to be ensured to be reduced to 1 multiplied by 10 during the vacuum magnetron sputtering -4 ～8×10 -4 Sputtering is started at Pa;
step two, sputtering deposition of titanium doped tungsten oxide layer
Sputtering a titanium doped tungsten oxide target material on the cleaned FTO glass layer to obtain a titanium doped tungsten oxide layer, wherein the titanium doped tungsten oxide target material contains less than or equal to 5 mass percent of titanium, the deposition rate is 0.02+/-0.002 nm/s, and the deposition thickness is 30-40 nm;
step three, tungsten oxide conformal crystallization
Placing the FTO glass layer with the titanium doped tungsten oxide layer into a muffle furnace for heat treatment, wherein the heating rate is 3-5 ℃/min, and when the temperature is raised to 400-500 ℃, preserving heat for 2-3 h, and naturally cooling to room temperature to obtain the heat treated titanium doped tungsten oxide layer;
step four, depositing a metal film
Sputtering and depositing a metal film on the surface of the titanium doped tungsten oxide layer after heat treatment, wherein the deposition rate is 0.03+/-0.002 nm/s, and the deposition thickness is 20-30 nm; the detector structure of the metal/titanium doped tungsten oxide Schottky junction is manufactured.
In the third step, the surface of the titanium doped tungsten oxide layer after heat treatment presents a conformal structure with high and low fluctuation so as to obtain a morphology with larger specific surface area, a surface plasmon effect is generated, and preparation is made for obviously improving the effective area of a Schottky junction formed by subsequent metal deposition. This is a feature of the invention.
In the fourth step, when the thickness of the metal film is unlimited, a vacuum evaporation method can be used for replacing sputtering deposition to obtain a metal film layer, the vacuum evaporation current is 120A, and the time is 1-2s, so that the detector structure of the metal/titanium doped tungsten oxide Schottky junction is obtained.
In the fourth step, the detector structure of the metal/titanium doped tungsten oxide schottky junction is used for preparing a photoelectric detector device, and the detection wavelength is as follows: 350nm-1100nm, effective receiving area: 36-100mm 2 Response time: 1-5 mu s of the total length of the glass,working temperature range: -dark current at 10-70 ℃): 1X 10 -8 ～5×10 -11 A, signal output mode: current, light absorption: 53-57%.
In the fourth step, the prepared photodetector device can particularly absorb near infrared light (750 nm-1100 nm), and the light absorptivity is preferably 56-57%.
In the fourth step, a plasmon effect is generated in the photoelectric detection process of the detector structure of the metal/titanium doped tungsten oxide Schottky junction.
The invention has the beneficial effects that:
the invention has the advantages of low cost, easy preparation and stable device performance. The metal layer with the conformal structure is formed to excite the surface plasmon effect of the device, so that the absorption efficiency of the device on incident light is enhanced, the sensitivity is improved, the response spectrum of the device is widened, the wide spectrum photoelectric detection rudiment device with higher performance is further obtained, the light absorption efficiency of 53-57% can be maintained in the wide spectrum range of 350-1100 nm correspondingly, the detection on near infrared light can be realized, the high-efficiency stable light absorption in the whole visible light and near infrared region is realized, the band gap width of a semiconductor is not limited, and the device is greatly improved compared with the traditional inorganic material detector.
The device can effectively slow down the relaxation process of electrons, reduce energy loss and improve the energy conversion efficiency of the photoelectric detector; in a doped semiconductor plasmon material system, the hot electron transfer is two orders of magnitude faster than that of a common device, and the photoelectric response speed can be effectively improved.
Description of the drawings:
figure 1 is a schematic diagram of the structure of a metal/titanium doped tungsten oxide schottky junction detector according to the present invention,
1-FTO glass layer, 2-titanium doped tungsten oxide layer, 3-metal film layer;
fig. 2 is an SEM image of a sample titanium-doped tungsten oxide layer obtained in inventive example 4, fig. 2 (a) is an SEM image of a sample titanium-doped tungsten oxide layer not subjected to heat treatment, fig. 2 (b) is an SEM image of a sample 400 ℃ heat-treated titanium-doped tungsten oxide layer, fig. 2 (c) is an SEM image of a sample 450 ℃ heat-treated titanium-doped tungsten oxide layer, and fig. 2 (d) is an SEM image of a sample 500 ℃ heat-treated titanium-doped tungsten oxide layer;
FIG. 3 shows XRD patterns of a sample titanium doped tungsten oxide layer obtained in example 4 of the present invention, and (a) shows XRD patterns of a titanium doped tungsten oxide layer which is not heat treated; (b) XRD patterns of the titanium doped tungsten oxide layer subjected to heat treatment at 450 ℃;
FIG. 4 is an absorption spectrum of a detector structure of a metal/titanium doped tungsten oxide Schottky junction prepared in example 4 of the present invention at a wavelength of 350nm-1100 nm;
fig. 5 is a graph of the transient light response of the detector structure of the metal/titanium doped tungsten oxide schottky junction prepared in example 4 of the present invention.
The specific embodiment is as follows:
the present invention will be described in further detail with reference to examples.
The materials used in the invention include:
high-purity gold target, high-purity aluminum target, aluminum strip, tungsten-titanium alloy target, FTO conductive glass, absolute ethyl alcohol and acetone.
The dosage of each material is as follows:
gold target: au 60 x 3mm
And (3) an aluminum target: al 60 x 3mm
Aluminum strip: 7g
Tungsten titanium alloy target: 60mm 5mm, titanium content below 5%
Deionized water: h 2 O 2500±50ml
Acetone: 70+ -5 ml
Ethanol: 200+ -10 ml
FTO conductive glass: 14mm
The preparation method of the detector structure of the metal/titanium doped tungsten oxide Schottky junction comprises the following steps:
(1) Selecting a high purity chemical
Selecting chemical preparations required by a preparation process, and specifically selecting analytically pure reagents for preparation;
(2) Pretreatment of FTO conductive glass
1) Wearing disposable gloves, repeatedly rubbing the front side, the back side and the side surfaces of the conductive glass with deionized water, clamping alcohol cotton by using tweezers, rubbing the surface of the conductive glass, checking by light until no macroscopic stains exist on the surface;
2) Placing the FTO conductive glass into an ultrasonic cleaner, adding acetone, and ultrasonically cleaning for 10min;
3) Placing the FTO conductive glass into an ultrasonic cleaner, adding absolute ethyl alcohol, and ultrasonically cleaning for 10min;
4) Placing the FTO conductive glass into an ultrasonic cleaner, adding deionized water, and ultrasonically cleaning for 10min;
5) And (3) placing the FTO conductive glass cleaned by the ultrasonic cleaner into a constant-temperature oven for drying, wherein the temperature of the constant-temperature oven is set to be 70 ℃.
6) And placing the dried FTO conductive glass into an oxygen plasma cleaner for cleaning for 8min.
(3) Magnetron sputtering equipment, muffle furnace and vacuum evaporator machine for preparing hot electron photoelectric detection embryonic device
1) The preparation is carried out in a vacuum chamber of a magnetron sputtering instrument;
2) Placing conductive glass
Firstly, opening a valve to balance the air pressure in the vacuum chamber with the atmospheric pressure; then opening the vacuum chamber, fixing the cleaned glass sample on a turntable at the top of the vacuum chamber, and leading the fluorine-doped tin oxide surface of the conductive glass to face downwards;
3) Placing a tungsten-titanium alloy target with the size of 60mm 5mm on the radio frequency sputtering target;
4) Lowering the upper cover of the vacuum chamber and closing the vacuum chamber;
5) Starting a mechanical vacuum pump, a composite vacuum gauge, a molecular vacuum pump and a gate valve, and pumping air in a vacuum chamber to ensure that the vacuum degree in the furnace is 1 multiplied by 10 -4 ～8×10 -4 Pa, and opening preheating;
6) Opening an oxygen ventilation switch, and adjusting the oxygen inlet flow to 20-40 sccm;
7) Regulating the gate valve in the closing direction until reaching the required vacuum degree, regulating the current and the voltage, and controlling the output power;
8) Preparing a titanium doped tungsten oxide semiconductor layer:
aligning conductive glass with a radio frequency sputtering target, opening a sputtering target position baffle, starting a radio frequency power switch, adjusting the sputtering power to 100-120W, enabling the surface of the target to glow, pre-sputtering for 10-15 min, closing the corresponding target position baffle, starting sputtering, and enabling the thickness of a deposited film layer to be 30-40 nm, wherein the deposition rate is 0.02+/-0.002 nm/s;
9) After sputtering, the baffle is opened, the current and voltage switch of the target position is closed, the air valve and the air bottle are closed, and after film deposition is completed in a vacuum state, the device is allowed to stand in the vacuum chamber for cooling for 30min;
10 High temperature annealing:
placing the FTO conductive glass with the titanium doped tungsten oxide layer deposited by magnetron sputtering into a muffle furnace, performing high-temperature annealing in an air state, adjusting the temperature rising rate to 4 ℃ per minute, rising the temperature to 400-500 ℃, keeping the temperature for 2-3 h, and naturally cooling to room temperature to realize the conformal crystallization of the titanium doped tungsten oxide, and increasing the surface area.
11 Sputtering or evaporating film electrode):
placing a gold target (aluminum target) with the size of 60mm x 3mm on the direct current sputtering target; repeating the operations 4) to 7), wherein the gas introduced in the operation 6) is regulated to argon, and the ventilation flow is 20-40 sccm; aligning conductive glass with a direct current sputtering target, adjusting current and voltage according to output power, opening a sputtering target position baffle, starting a direct current sputtering power switch, adjusting sputtering power to 15-25W, maintaining the sputtering rate to be 0.03+/-0.002 nm/s, pre-sputtering for 10-15 min, closing a corresponding target position baffle, starting sputtering, and depositing a film layer with the thickness of 20-30 nm;
if a vacuum evaporation method is adopted, firstly putting on gloves, cutting an aluminum sheet into small strips by scissors, respectively carrying out ultrasonic cleaning for 10min by using propanol, deionized water and alcohol, and then drying in a drying oven; adhering a sample to a grinding plate, placing an aluminum strip on a tungsten wire, and closing the top of an evaporation chamber cover; sequentially opening a mechanical pump, a backing valve, circulating water, a molecular pump and an evaporation power switch; when the vacuum is pumped to 3.8X10 -3 When Pa, switching on an inverter evaporation power supply and starting, quickly rotating the current to be 120A, stopping for 1s, quickly rotating to be 0, and ending evaporation;
12 Standing and cooling along with the cavity in a vacuum state:
after the film deposition is completed, the photoelectric detector is kept stand and cooled for 30min in a vacuum chamber;
if the vapor deposition mode is adopted, closing the molecular pump after the vapor deposition is finished, waiting for the rotating speed of the molecular pump to be 0, then sequentially closing circulating water, a vapor deposition power supply, a mechanical pump, a backing valve and a total power supply, and standing for 30min;
13 Collecting the product: rudiment device of gold (aluminum)/tungsten oxide schottky junction for photoelectric detection
Sequentially closing the molecular vacuum pump and the mechanical vacuum pump;
opening an air inlet valve;
opening a cabin door of the vacuum cabin;
if the evaporation mode is adopted, a main power supply and a deflation valve are opened, and a sample is taken out; closing the total power supply;
and taking out the prepared hot electron photoelectric detection embryonic device, namely the detector structure of the metal/titanium doped tungsten oxide Schottky junction, and the structural schematic diagram is shown in figure 1.
14 Quality detection, device characterization
Performing quality detection and characterization of the device performance on the prepared photoelectric detection embryonic device, and measuring the XRD spectrum of the titanium doped tungsten oxide sample by adopting an X-ray diffractometer; observing the surface morphology of the device with a scanning electron microscope; in terms of performance characterization: testing the absorption spectrum of the device by using an ultraviolet-visible near-infrared spectrophotometer; the device was tested for its bright-dark current response curve at 0V bias using an ultraviolet visible near infrared spectrophotometer in combination with a Keithley digital source meter.
Specifically, the gold (aluminum) film and the titanium doped tungsten oxide layer of the photoelectric detector have different thicknesses, and correspondingly have different parameter settings in the preparation process, and the method specifically comprises the following steps:
example 1
Firstly, performing step (2), namely fixing the FTO conductive glass on a sample support after cleaning, wherein the conductive side (namely the FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and tightly closing an upper cover of a vacuum chamber;
operations 3) to 9) in step (3) were performed, and the tungsten-titanium alloy target used in this example was used in a ratio of Ti: wo=2.5:97.5, in which the vacuum in the chamber was evacuated to 5×10 -4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium-doped tungsten oxide semiconductor layer on the FTO glass;
and (3) taking out the sample after cooling, placing the sample in a muffle furnace, performing heat treatment for 2.5 hours at the temperature of 400 ℃ to obtain a titanium doped tungsten oxide layer with the surface exhibiting a conformal structure after heat treatment, and naturally cooling along with the furnace.
And (3) placing the heat-treated sample in a thermal evaporation device, placing an aluminum wire, and performing sputtering deposition operation in the steps (3) 11) to 13), so as to form an aluminum film on the surface of the titanium-doped tungsten oxide layer of the sample, thereby obtaining the detector structure of the aluminum/titanium-doped tungsten oxide Schottky junction.
Example 2
Firstly, performing step (2), and cleaning FTO conductive glass; fixing the glass on a sample support, wherein one conductive side (namely an FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and closing an upper cover of a vacuum chamber;
performing operations 3) to 9) in step (3), the proportion of the tungsten-titanium alloy target used in this example being the same as that in example 1, wherein the vacuum in the chamber was evacuated to 5X 10 -4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium-doped tungsten oxide semiconductor layer on the FTO glass;
and (3) taking out the sample after cooling, placing the sample in a muffle furnace, performing heat treatment for 2.5 hours at the temperature of 425 ℃ to obtain a titanium doped tungsten oxide layer with the surface exhibiting a conformal structure after heat treatment, and naturally cooling along with the furnace.
And (3) placing the heat-treated sample in a thermal evaporation device, placing an aluminum wire, and performing sputtering deposition operation in the steps (3) 11) to 13), so as to form an aluminum film on the surface of the titanium-doped tungsten oxide layer of the sample, thereby obtaining the detector structure of the aluminum/titanium-doped tungsten oxide Schottky junction.
Example 3
Firstly, performing step (2), and cleaning FTO conductive glass; fixing the glass on a sample support, wherein one conductive side (namely an FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and closing an upper cover of a vacuum chamber;
operations 3) to 9) in step (3) were performed, and the tungsten-titanium alloy target used in this example was used in a ratio of 3.4:96.6, in which the vacuum in the chamber was evacuated to 5×10 -4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium-doped tungsten oxide semiconductor layer on the FTO glass;
and (3) taking out the sample after cooling, placing the sample in a muffle furnace, performing heat treatment for 2.5 hours at the temperature of 450 ℃ to obtain a titanium doped tungsten oxide layer with the surface exhibiting a conformal structure after heat treatment, and naturally cooling along with the furnace.
And (3) placing the heat-treated sample in a thermal evaporation device, placing an aluminum wire, and performing sputtering deposition operation in the steps (3) 11) to 13), so as to form an aluminum film on the surface of the titanium-doped tungsten oxide layer of the sample, thereby obtaining the detector structure of the aluminum/titanium-doped tungsten oxide Schottky junction.
Example 4
Firstly, performing step (2), and cleaning FTO conductive glass; fixing the glass on a sample support, wherein one conductive side (namely an FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and closing an upper cover of a vacuum chamber;
operations 3) to 9) in step (3) were performed, and the tungsten-titanium alloy target used in this example was used in a ratio of 4.4:95.6, in which the vacuum in the chamber was evacuated to 5×10 -4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium-doped tungsten oxide semiconductor layer on the FTO glass;
taking out the sample after cooling, equally dividing the sample into four samples, and respectively performing non-heat treatment and heat treatment at different temperatures of 400 ℃,450 ℃ and 500 ℃, wherein the heating time at 400 ℃ is 3 hours, the heating time at 450 ℃ is 2.5 hours, and the heating time at 500 ℃ is 2 hours; and naturally cooling along with a furnace after heating to obtain an untreated titanium doped tungsten oxide film, a titanium doped tungsten oxide film heat-treated at 400 ℃, a titanium doped tungsten oxide film heat-treated at 450 ℃ and a titanium doped tungsten oxide film heat-treated at 500 ℃, obtaining four groups of different samples, and placing the four groups of samples in a muffle furnace to heat-treat for 2.5 hours at 450 ℃.
The SEM image of the sample titanium doped tungsten oxide layer is shown in fig. 2, wherein fig. 2 (a) is an SEM image of the sample non-heat treated titanium doped tungsten oxide layer, fig. 2 (b) is an SEM image of the sample 400 ℃ heat treated titanium doped tungsten oxide layer, fig. 2 (c) is an SEM image of the sample 450 ℃ heat treated titanium doped tungsten oxide layer, and fig. 2 (d) is an SEM image of the sample 500 ℃ heat treated titanium doped tungsten oxide layer, as can be seen from fig. 2 (a), the tungsten oxide film is compact and flat and almost free of impurities, because the magnetron sputtering technology can generate a uniform and flat film layer; as can be seen from fig. 2 (b), 2 (c) and 2 (d), the tungsten oxide is crystallized in a conformal manner and then is closely packed in a granular shape, an invagination structure is formed on the surface of the film, the appearance of high and low fluctuation appears, the conformal characteristic is realized, and the effect of enhancing the plasma primitive element by the metal on the surface of the final device is facilitated. Among them, the effect of the titanium doped tungsten oxide layer heat treated at 450 ℃ is more outstanding.
The XRD pattern of the titanium doped tungsten oxide layer of the sample is shown in figure 3, wherein the figure 3 (a) is the XRD pattern of the titanium doped tungsten oxide layer which is not subjected to heat treatment, and as can be seen from the figure, no obvious characteristic peak exists, and the fluctuation of intensity is not as slow as that of the XRD pattern after heat treatment; the graph 3 (b) is an XRD graph of the titanium doped tungsten oxide layer after heat treatment at 450 ℃, and obvious characteristic peaks are obvious when 2θ=23.96 °, 34.05 ° and 55.26 °.
And (3) placing the heat-treated sample in a vacuum magnetron sputtering device, placing an aluminum wire, and then performing sputtering deposition operation in steps (3) 11) to 13), so as to form an aluminum film on the surface of the titanium-doped tungsten oxide layer of the sample. The detector structure of the aluminum-titanium doped tungsten oxide Schottky junction is obtained, and the structure can obtain a complete photoelectric detector device through a device assembly process compatible with or completely consistent with a traditional photoelectric detector. The light absorption spectrum of the device at the wavelength of 350-1100 nm is shown in fig. 4, through the absorption spectrum, the device can keep the average light absorption of 57% in the wavelength of 350-1100 nm, compared with pure tungsten oxide and tungsten oxide which is not subjected to heat treatment, the light absorption and photoelectric detection capability of the device are obviously improved, the device can particularly realize the absorption of near infrared light (750-1100 nm), and the tungsten oxide can not detect the light in the range due to the limitation of the forbidden bandwidth. The device prepared by the invention has an invagination structure as shown in the figure 2, can excite the surface plasmon effect, has higher photovoltaic acquisition capacity, and can realize detection of the semiconductor on non-absorption wave band light. A typical optical response spectrum of the structural device at 350-1100 nm is shown in fig. 5, and it can be seen that the structural device can generate specific current signals for optical signals with specific wavelengths in the near ultraviolet band to the near infrared band, and the signals can be kept stable and can be directly used for optical signal detection to prepare the detector structure of the aluminum/titanium doped tungsten oxide Schottky junction.
Example 5
Firstly, performing step (2), and cleaning FTO conductive glass; fixing the glass on a sample support, wherein one conductive side (namely an FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and closing an upper cover of a vacuum chamber;
performing operations 3) to 9) in step (3) using the same ratio of the tungsten-titanium alloy target as in example 4, wherein the vacuum in the chamber was evacuated to 5X 10 -4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium-doped tungsten oxide semiconductor layer on the FTO glass;
and (3) taking out the sample after cooling, placing the sample in a muffle furnace, performing heat treatment for 2.5 hours at the temperature of 500 ℃ to obtain a titanium doped tungsten oxide layer with the surface exhibiting a conformal structure after heat treatment, and naturally cooling along with the furnace.
And (3) placing the heat-treated sample in a magnetron sputtering device, placing an aluminum target, and performing sputtering operations in the steps (3) 11) to 13), so as to form an aluminum film on the surface of the titanium-doped tungsten oxide layer of the sample, thereby obtaining the detector structure of the aluminum/titanium-doped tungsten oxide Schottky junction.
Example 6
Firstly, performing step (2), and cleaning FTO conductive glass; fixing the glass on a sample support, wherein one conductive side (namely an FTO layer) faces outwards, placing the sample support into a sample rotating table, adjusting the position, and then descending and closing an upper cover of a vacuum chamber;
operations 3) to 9) in step (3) were performed, and the tungsten-titanium alloy target used in this example was used in a ratio of 5.0:95.0, in which the vacuum in the chamber was evacuated to 5×1 0-4 Opening an oxygen cylinder air valve after Pa, and adjusting the oxygen flow to 20sccm; in the sputtering process, controlling the output power of a magnetron sputtering instrument to be 100W, and starting formal sputtering after pre-sputtering for 10min to generate a titanium doped tungsten oxide semiconductor layer on the FTO glass, wherein the thickness is 40nm;
and (3) taking out the sample after cooling, placing the sample in a muffle furnace, performing heat treatment for 2.5 hours at the temperature of 500 ℃ to obtain a titanium doped tungsten oxide layer with the surface exhibiting a conformal structure after heat treatment, and naturally cooling along with the furnace.
And (3) placing the heat-treated sample in a thermal evaporation device, placing an aluminum wire, and then performing evaporation operation in the steps (3) 11) to 13), wherein an aluminum film is formed on the surface of the titanium-doped tungsten oxide layer of the sample, and the thickness is 30nm, so that the detector structure of the aluminum/titanium-doped tungsten oxide Schottky junction is manufactured.
The detector structure of the aluminum/titanium doped tungsten oxide schottky junction prepared in the above embodiment adopts a conventional process to prepare a complete photoelectric detector device, and a light absorption experiment is performed, and the photoelectric detector device obtained by the detector structures prepared in examples 1-5 can particularly realize the absorption of near infrared light (750 nm-1100 nm). The performance of the devices of the examples after instrument characterization is shown in table 1 below:
TABLE 1
In the above table, the thickness of the aluminum film and the thickness of the titanium tungsten layer are in nm, and the heat treatment temperature is in DEG CThe space is h, the wavelength range is nm, and the effective receiving area is mm 2 Response time is in mus and dark current is in a.

Claims (6)

1. The detector structure of the metal/titanium doped tungsten oxide Schottky junction is characterized by comprising an FTO glass layer, a titanium doped tungsten oxide layer and a metal film layer from bottom to top, wherein the thickness of the FTO glass layer is 200-nm, the thickness of the titanium doped tungsten oxide layer is 30-40 nm, the metal is gold or aluminum, the thickness of the metal film layer is 20-30 nm, and the mass percentage of titanium in the titanium doped tungsten oxide layer is less than or equal to 5%; the detector structure of the metal/titanium doped tungsten oxide Schottky junction is used for photoelectric detection, and the detection wavelength is as follows: 350nm-1100nm, effective receiving area: 36-100mm 2 Response time: 1-5 mu s, working temperature range: -dark current at 10-70 ℃): 1X 10 -8 ~5×10 -11 A, signal output mode: current, light absorption: 53-57%;
the surface of the titanium doped tungsten oxide layer presents a conformal structure with high and low fluctuation.
2. The detector structure of claim 1, wherein the titanium doped tungsten oxide layer comprises 2.5-5% titanium by mass.
3. The method of fabricating a metal/titanium doped tungsten oxide schottky junction detector structure of claim 1 comprising the steps of:
step one, FTO glass layer treatment
Taking the FTO glass layer as a substrate, and performing secondary cleaning after primary cleaning and drying;
step two, sputtering deposition of titanium doped tungsten oxide layer
Sputtering a titanium-doped tungsten oxide target on the cleaned FTO glass layer to obtain a titanium-doped tungsten oxide layer with the thickness of 30-40 nm;
step three, tungsten oxide conformal crystallization
Placing the FTO glass layer with the titanium-doped tungsten oxide layer into a muffle furnace for heat treatment, wherein the heating rate is 3-5 ℃/min, and when the temperature is raised to 400-500 ℃, preserving heat for 2-3 h, and naturally cooling to room temperature to obtain the heat-treated titanium-doped tungsten oxide layer; the surface of the titanium doped tungsten oxide layer after heat treatment presents a conformal structure with high and low fluctuation, a surface plasmon effect appears, the contact surface area with the metal of magnetron sputtering is increased, and the effective area for forming a Schottky junction structure is increased;
step four, depositing a metal film
Sputtering and depositing a metal film on the surface of the titanium doped tungsten oxide layer after heat treatment, wherein the deposition rate is 0.03+/-0.002 nm/s, and the deposition thickness is 20-30 nm; the detector structure of the metal/titanium doped tungsten oxide Schottky junction is manufactured.
4. The method for manufacturing a detector structure of a metal/titanium doped tungsten oxide schottky junction according to claim 3, wherein in the first step, the primary cleaning mode is that deionized water, absolute ethyl alcohol and acetone are sequentially used for ultrasonic cleaning in an ultrasonic cleaning machine for 10-15 min respectively; drying operation and constant temperature oven, wherein the drying temperature is 60-80 ℃, and the secondary cleaning is performed in a plasma cleaning machine for 6-8min; the sputtering mode is vacuum magnetron sputtering, and the pressure in the vacuum chamber of the magnetron sputtering needs to be ensured to be reduced to 1 multiplied by 10 during the vacuum magnetron sputtering -4 ~8×10 -4 Sputtering starts at Pa.
5. The method of fabricating a metal/titanium doped tungsten oxide schottky junction detector structure according to claim 3, wherein in the second step, the sputter deposition rate of the titanium doped tungsten oxide target is 0.02±0.002nm/s.
6. The method of fabricating a metal/titanium doped tungsten oxide schottky junction detector structure according to claim 3, wherein in the third step, the heating rate of the heat treatment is 3-5 ℃/min.
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