CN111816715A - Zinc oxide nanowire array ultraviolet detector and preparation method thereof - Google Patents
Zinc oxide nanowire array ultraviolet detector and preparation method thereof Download PDFInfo
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- H01L31/0264—Inorganic materials
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Abstract
The invention provides a zinc oxide nanowire array ultraviolet detector and a preparation method thereof. The zinc oxide nanowire array ultraviolet detector provided by the invention comprises: the device comprises a substrate and a zinc oxide nanowire array layer compounded on the surface of the substrate; the surface of the zinc oxide nanowire array layer sequentially comprises a first electrode area, a non-electrode area and a second electrode area along the length direction; electrodes are compounded on the first electrode area and the second electrode area; indium particles are fixed on the electrodes; the non-electrode area is compounded with a modification layer; the modification layer is a fluorine-silicon-based modification layer; the fluorine-silicon-based modification layer comprises: SiF4And F. F and are carried out on the surface of the zinc oxide nanowire array layer in a non-electrode areaSiF4The double modification can effectively reduce the dark current of the ultraviolet detector, improve the responsivity and reduce the response time.
Description
Technical Field
The invention relates to the technical field of semiconductor devices, in particular to a zinc oxide nanowire array ultraviolet detector and a preparation method thereof.
Background
An ultraviolet detector is a sensor that converts one form of electromagnetic radiation signal into another form that can be easily processed, such as a photodetector that converts optical radiation into an electrical signal using the photoelectric effect. Therefore, the ultraviolet detector can be applied to many fields, such as fire early warning, missile tail flame detection, military communication, biological effect, environmental monitoring and the like.
Currently, commercial ultraviolet detector types are mainly photomultiplier tubes, silicon detectors and semiconductor detectors. The photomultiplier needs to work under high voltage, and has low efficiency, heavy volume, easy damage and higher cost; the silicon-based ultraviolet phototube needs an additional optical filter, so that the cost is high and the carrying is inconvenient; both have certain limitations in practical applications. In contrast, semiconductor materials have the advantages of portability, low cost, high responsivity, and the like, and thus are receiving much attention.
Currently, most studied semiconductor materials mainly comprise AlGaN alloy of III-V group and MgZnO alloy of II-VI group. The currently reported GaN can be used for widening an energy band to a solar blind area by doping aluminum, and is made into detectors with structures such as MSM (metal-semiconductor-metal) and p-n. However, the growth temperature of AlGaN is high, and the alloy crystal quality of the high aluminum component is poor. ZnO as another wide-bandgap semiconductor has the advantages of strong radiation resistance, high electron saturation drift velocity, matched single crystal substrate, easy synthesis, no toxicity, no harm, rich resources, environmental friendliness and the like, and is one of candidate materials for preparing wide-bandgap ultraviolet detectors.
The three most important parameters for an ultraviolet detector are the responsivity of the device, the dark current and the response time. Responsivity and dark current determine the sensitivity of the device and the detection capability of the device on weak signals, and the higher the responsivity is, the better the responsivity is, and the lower the dark current is, the better the dark current is. The response time determines the rapid signal discrimination capability of the device, the requirement on the response time in the fields of ultraviolet alarm and ultraviolet communication is higher, and the faster the response time is, the better the response time is. Therefore, how to improve the performance is a key in the development of the ultraviolet detector. The existing improvement method is generally difficult to simultaneously optimize the three important parameters; especially with respect to the response time of the device, it is difficult to further improve, possibly even with a concomitant reduction in the responsivity of the device.
Disclosure of Invention
In view of this, the present invention aims to provide a zinc oxide nanowire array ultraviolet detector and a preparation method thereof. The zinc oxide nanowire array ultraviolet detector provided by the invention can effectively and simultaneously improve the effects of three aspects of responsivity, dark current and response time.
The invention provides a zinc oxide nanowire array ultraviolet detector, which comprises:
the device comprises a substrate and a zinc oxide nanowire array layer compounded on the surface of the substrate;
the surface of the zinc oxide nanowire array layer sequentially comprises a first electrode area, a non-electrode area and a second electrode area along the length direction;
electrodes are compounded on the first electrode area and the second electrode area; indium particles are fixed on the electrodes;
the non-electrode area is compounded with a modification layer;
the modification layer is a fluorine-silicon-based modification layer; the fluorine-silicon-based modification layer comprises: SiF4And F.
Preferably, the thickness of the zinc oxide nanowire array layer is 50-1000 nm;
the thickness of the electrode is 5-300 nm.
Preferably, the electrode is a gold electrode or a gold-nickel alloy electrode.
Preferably, the electrodes are in the shape of bulk electrodes or interdigital electrodes.
Preferably, the distance between the first electrode area and the second electrode area is 0.2-2 mm.
Preferably, the inter-finger distance of the interdigital electrodes is 1-10 mu m, the interdigital length is 0.1-2 mm, the interdigital width is 1-10 mu m, and the number of the interdigital electrodes in each electrode is 10-100.
The invention also provides a preparation method of the zinc oxide nanowire array ultraviolet detector in the technical scheme, which comprises the following steps:
a) growing a zinc oxide nanowire array layer on the surface of the substrate to obtain a complex A;
b) placing a shelter in the center of the zinc oxide nanowire array layer, and sequentially dividing the surface of the zinc oxide nanowire array layer into a first electrode area, a non-electrode area and a second electrode area along the length direction; forming electrodes on the first electrode area and the second electrode area to obtain a composite body B;
c) growing SiO in the non-electrode area of the zinc oxide nanowire array layer in the compound B2Modifying the layer to obtain a composite C;
d) for SiO on the composite C2And carrying out fluorine modification treatment on the modification layer to form a fluorine-silicon-based modification layer, and fixing indium particles on the electrode to obtain the ultraviolet detector.
Preferably, the step d) comprises:
placing the compound C above a fluorine solution in the air, wherein the SiO is2The modification layer faces the fluorine solution; and heating the fluorine solution to form a fluorine-silicon-based modification layer on the zinc oxide nanowire array layer.
Preferably, the fluorine solution is one or more of an HF solution, a KF solution, a NaF solution, a trifluoroacetic acid solution, a trifluoromethanesulfonic acid solution and a trifluoropropionic acid solution.
Preferably, the fluorine concentration in the fluorine solution is 1 × 10-6mol/L～10mol/L；
The height of the suspension is 0.1-50 cm;
the temperature of the temperature rise is 25-100 ℃, and the heat preservation treatment time after the temperature rise is 0.01 s-24 h.
Compounding a zinc oxide nanowire array layer on a substrate, and dividing the zinc oxide nanowire array layer into three regions along the length direction, wherein the three regions are a first electrode region, a non-electrode region and a second electrode region respectively; electrodes are respectively arranged on the first electrode area and the second electrode area at two ends of the zinc oxide nanowire array layer, and indium grains are fixed on the electrodes;compounding a modification layer in a non-electrode region between a first electrode region and a second electrode region, wherein the modification layer is F and SiF4And (4) a double modification layer. Through the specific modification layer, the dark current of the ultraviolet detector can be effectively reduced, the responsivity is improved, and the response time is shortened.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an ultraviolet detector provided by the present invention;
FIG. 2 is a schematic diagram of surface area division of a zinc oxide nanowire array layer;
FIG. 3 is a schematic flow chart of a method for manufacturing the ultraviolet detector provided by the present invention;
fig. 4 is an SEM image of the zinc oxide nanowire array layer formed in example 1;
FIG. 5 is a graph of I-V curves before and after modification of the UV detector;
FIG. 6 is a graph of the light response before and after modification of the UV detector;
FIG. 7 is a graph of response time before and after modification of the UV detector.
Detailed Description
The invention provides a zinc oxide nanowire array ultraviolet detector, which comprises:
the device comprises a substrate and a zinc oxide nanowire array layer compounded on the surface of the substrate;
the surface of the zinc oxide nanowire array layer sequentially comprises a first electrode area, a non-electrode area and a second electrode area along the length direction;
electrodes are compounded on the first electrode area and the second electrode area; indium particles are fixed on the electrodes;
the non-electrode area is compounded with a modification layer;
the modification layer is a fluorine-silicon-based modification layer; the fluorine-silicon-based modification layer comprises: SiF4And F.
Compounding a zinc oxide nanowire array layer on a substrate, and dividing the zinc oxide nanowire array layer into three regions along the length direction, wherein the three regions are a first electrode region, a non-electrode region and a second electrode region respectively; electrodes are respectively arranged on the first electrode area and the second electrode area at two ends of the zinc oxide nanowire array layer, and indium grains are fixed on the electrodes; compounding a modification layer in a non-electrode region between a first electrode region and a second electrode region, wherein the modification layer is F and SiF4And (4) a double modification layer. Through the specific modification layer, the dark current of the ultraviolet detector can be effectively reduced, the responsivity is improved, and the response time is shortened.
Referring to fig. 1, fig. 1 is a schematic structural diagram of an ultraviolet detector provided by the present invention, wherein 1 is a substrate, 2 is a zinc oxide nanowire array layer, 3 is an electrode, 4 is indium particles, and 5 is a fluorine-silicon-based modification layer.
The substrate 1 is a base material of the ultraviolet detector, and the kind thereof is not particularly limited, and may be a conventional substrate well known to those skilled in the art. In the present invention, the substrate 1 is preferably sapphire, quartz, or a substrate having a surface provided with SiO2A Si sheet of the layer. The specification of the substrate 1 is not particularly limited, and may be a conventional specification of a substrate in an ultraviolet detector, and in some embodiments of the present invention, the substrate specification is: the thickness is 0.5mm, and the length and the width are both 1 cm.
The zinc oxide nanowire array layer 2 is arranged on the substrate 1, and the length and the width of the zinc oxide nanowire array layer are preferably the same as those of the substrate 1, namely the zinc oxide nanowire array layer covers the substrate 1 completely. The invention provides a zinc oxide nanowire array-based ultraviolet detector on a substrate, namely the zinc oxide nanowire array-based ultraviolet detector is provided, and the ultraviolet detectors in different types or material forms have incomparable performance. In the invention, the thickness of the zinc oxide nanowire array layer 2 is preferably 50-1000 nm.
The surface of the zinc oxide nanowire array layer 2 sequentially comprises a first electrode area, a non-electrode area and a second electrode area along the length direction; referring to fig. 2, fig. 2 is a schematic diagram of surface area division of the zinc oxide nanowire array layer, wherein a first electrode area and a second electrode area are respectively located at two ends of the zinc oxide nanowire array layer, a non-electrode area is sandwiched between the two electrode areas, and the width of the non-electrode area is the distance between the first electrode area and the second electrode area. In the invention, the distance between the first electrode area and the second electrode area is preferably 0.2-2 mm.
The first electrode area and the second electrode area are respectively combined with an electrode 3. The electrode 3 is preferably a gold electrode or a gold-nickel alloy electrode. The structure of the electrode 3 is preferably a dense block electrode or an interdigital electrode, more preferably an interdigital electrode. The thickness of the electrode is preferably 5-300 nm. Wherein, for the compact block electrode, the shape can be cube, cuboid or cylinder. For the interdigital electrodes, the specifications thereof are preferably: the finger spacing is 1-10 mu m, the length of the interdigital is 0.1-2 mm, the width of the interdigital is 1-10 mu m, and the number of the interdigital in each electrode is 10-100.
Indium particles are fixed on the electrodes 3. The indium particles are preferably cylindrical in shape. The specification of the cylinder is preferably: the diameter is more than 0.5mm, and the contact area with the electrode is less than the area of the upper surface of the electrode; the height is 0.5-5 mm.
The non-electrode area is compounded with a modification layer; the modification layer is a fluorine-silicon-based modification layer; the fluorine-silicon-based modification layer comprises: SiF4And F. Firstly modifying SiO on the surface of the non-electrode area of the zinc oxide nanowire array layer 22Layer, further fluorine treatment, wherein F and SiO2React to form SiF4In addition, a part of F permeates through the loose SiO2 layer and reacts with the zinc oxide microwire in the inner layer, F is connected with Zn atoms in ZnO to form Zn-F bonds, and finally F and SiF are obtained4A modified zinc oxide nanowire array layer.
The specific conditions of the reaction between the F-containing substance and ZnO on the surface of the zinc oxide micron are as follows: surface of (1) ZnOZn-O dangling bonds exist, are unstable and can easily react with water vapor in the air to form Zn-OH, and the Zn-OH exists only on the surface in a trace amount, so that the chemical formula of ZnO is not influenced; when ZnO is brought into contact with a fluorine-containing species (in the case of HF), the following reaction Zn-OH + H takes place++F-→Zn-F+H2O, forming a Zn-F bond; ② the ZnO surface also has a bridging bond of Zn-O-Zn, and contacts with fluorine-containing substance (taking HF as an example) to react Zn-O-Zn +2H++2F-→2(Zn-F)+H2O, forming a Zn-F bond.
According to the invention, through the double-modification synergistic effect, the responsivity, the dark current and the response time of the detector can be effectively improved. In the prior art, the device performance is improved by pure fluorine modification, however, the applicant researches and discovers that if only fluorine modification is carried out on the zinc oxide nanowire array layer in the invention, the detector performance is reduced, and the fluorine modification and SiF are carried out4The modification is combined, and the performance of the detector can be effectively improved through double modification. In the invention, the modification layer is specifically compounded in the non-electrode area of the zinc oxide nanowire array layer.
The invention also provides a preparation method of the zinc oxide nanowire array ultraviolet detector in the technical scheme, which comprises the following steps:
a) growing a zinc oxide nanowire array layer on the surface of the substrate to obtain a complex A;
b) placing a shelter in the center of the zinc oxide nanowire array layer, and sequentially dividing the surface of the zinc oxide nanowire array layer into a first electrode area, a non-electrode area and a second electrode area along the length direction; forming electrodes on the first electrode area and the second electrode area to obtain a composite body B;
c) growing SiO in the non-electrode area of the zinc oxide nanowire array layer in the compound B2Modifying the layer to obtain a composite C;
d) for SiO on the composite C2And carrying out fluorine modification treatment on the modification layer to form a fluorine-silicon-based modification layer, and fixing indium particles on the electrode to obtain the ultraviolet detector.
Referring to fig. 3, fig. 3 is a schematic flow chart of a method for manufacturing an ultraviolet detector according to the present invention.
With respect to step a):
the kind, specification, etc. of the substrate are the same as those in the above technical solution, and are not described herein again. The preparation method of the zinc oxide nanowire array layer is preferably a molecular beam epitaxy method, a metal organic compound chemical vapor deposition method or a magnetron sputtering method. In some embodiments of the invention, metalorganic chemical vapor deposition (MOCVD) is employed; the method specifically comprises the following steps: putting the cleaned substrate into MOCVD growth equipment, controlling the growth temperature to be 500-800 ℃, and controlling the vacuum degree of a growth chamber to be 2 multiplied by 102～1×104Pa, adopting dimethyl zinc or diethyl zinc as a zinc source, leading the flow rate of carrier gas of a zinc source pipeline to be 5-20 mL/min, leading the flow rate of oxygen to be 100-1000 mL/min, and growing for 0.5-5 hours; forming a zinc oxide nanowire array film layer on the surface of the substrate. And then, closing the organic source, cooling at the cooling rate of 0.1-50 ℃/min, cooling to room temperature, and taking out the substrate to obtain the complex A compounded with the zinc oxide nanowire array layer.
With respect to step b):
placing a shelter in the center of the zinc oxide nanowire array layer, and sequentially dividing the surface of the zinc oxide nanowire array layer into a first electrode area, a non-electrode area and a second electrode area along the length direction; wherein, the mask corresponds to a non-electrode area, namely, the middle area of the zinc oxide nanowire array layer is covered, electrodes are respectively prepared in the electrode areas at the two sides of the mask area (corresponding to the non-electrode area), and after the preparation is finished, the mask is removed to form two electrodes which are not connected with each other, so as to obtain a complex B. Wherein, the interval area between the two electrodes is the non-electrode area.
In the present invention, the kind, structure, specification, etc. of the electrode are the same as those in the above technical solution, and are not described herein again. Wherein, the bulk electrode can be prepared by adopting a thermal evaporation method. For the interdigital electrode, a photoetching method can be adopted for preparation; the specific operation thereof is not particularly limited, and the interdigital electrodes may be formed according to a conventional method well known to those skilled in the art.
With respect to step c):
growing SiO in the non-electrode area of the zinc oxide nanowire array layer in the compound B2The specific method of modifying the layer preferably includes: placing the complex B in a magnetron sputtering device, and growing SiO in the non-electrode area of the zinc oxide nanowire array layer by using a magnetron sputtering method2And a finishing layer. The target material adopted by magnetron sputtering is preferably Si or SiO2(ii) a The sputtering atmosphere is oxygen; the sputtering temperature is 300-600 ℃; the sputtering power is 50-200W; the sputtering distance is 1-20 cm. After the sputtering treatment, a layer of loose SiO is formed in the non-electrode area of the zinc oxide nanowire array layer of the compound B2And (3) a layer. The SiO2The thickness of the layer is preferably 20 to 100 nm. After the modification treatment, the SiO-containing material is obtained2And a composite C of the decorative layers.
With respect to step d):
the process for performing the fluorine modification treatment specifically comprises: placing the compound C above a fluorine solution in the air, wherein the SiO is2The modification layer faces the fluorine solution; and heating the fluorine solution to form a fluorine-silicon-based modification layer on the zinc oxide nanowire array layer. Suspending the composite C above the fluorine solution, heating the fluorine solution to generate fluorine-containing vapor, F and SiO2React to form SiF4In addition, a part of F permeates through the loose SiO2 layer and reacts with the zinc oxide microwire in the inner layer, F is connected with Zn atoms in ZnO to form Zn-F bonds, and finally F and SiF are obtained4A modified zinc oxide nanowire array layer.
In the invention, the fluorine solution is preferably one or more of an HF solution, a KF solution, a NaF solution, a trifluoroacetic acid solution, a trifluoromethanesulfonic acid solution and a trifluoropropionic acid solution. The concentration of fluorine in the fluorine solution is preferably 1X 10-6mol/L～10mol/L。
In the invention, the hanging height is preferably 0.1-50 cm, and more preferably 0.1-20 cm; in some embodiments of the invention, the flying height is 0.1cm, 1cm, 5cm, 20cm, 30cm, or 50 cm. The suspension height refers to the height between the substrate and the surface of the fluorine solution.
In the invention, the temperature rise is preferably 25-100 ℃, and more preferably 40-80 ℃; in some embodiments of the invention, the elevated temperature is 40 ℃. After the temperature is raised to the target temperature, carrying out heat preservation treatment for a certain time; in the present invention, the time for the heat-retaining treatment is preferably 1s to 24 hours, more preferably 1s to 1 hour, even more preferably 1s to 5min, and most preferably 10 to 60 s. In some embodiments of the invention, the treatment time is 1s, 10s, 20s, 60s, 5min or 1 h. After the treatment, F and SiF are formed in the non-electrode area of the zinc oxide nanowire array layer4A modified fluorosilicone group modification layer.
In the present invention, after the fluorine modification treatment, it is preferable to further include: and (4) cleaning and drying. The washing is preferably with deionized water. The drying is preferably blow-dried with nitrogen.
In the present invention, indium particles are fixed to the two electrodes after the above-described treatment. The fixing manner is not particularly limited, and for example, indium particles can be directly pressed and fixed on the electrode. After the treatment, F and SiF are obtained4Modified double modified MSM (i.e. metal-semiconductor-metal) structure ultraviolet detector.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example 1
S1 growing zinc oxide nanowire array layer by MOCVD method
The sapphire substrate (specification of the substrate: thickness 0.5mm x length 1cm x width 1cm) was cleaned with trichloroethylene, acetone and ethanol, respectively, and then dried with dry nitrogen.
Putting the cleaned substrate into MOCVD growth equipment, controlling the growth temperature at 650 ℃, and controlling the vacuum degree of a growth chamber at 1 × 103Pa, adopting dimethyl zinc as a zinc source, leading the flow rate of carrier gas of a zinc source pipeline to be 10mL/min, leading the flow rate of oxygen to be 500mL/min, and growing for 3 hours; forming zinc oxide nano-particles on the surface of the substrateWire array thin film layer (thickness 400 nm). And then, closing the organic source, cooling to room temperature at a cooling rate of 10 ℃/min, and taking out the substrate to obtain a complex A compounded with the zinc oxide nanowire array layer.
Microstructure of the formed zinc oxide nanowire array layer referring to fig. 4, fig. 4 is an SEM image of the zinc oxide nanowire array layer formed in example 1.
S2 preparation of electrode
Placing a mask (the width is 100 mu m, the length is the same as the width of the zinc oxide nanowire array layer) in the center of the zinc oxide nanowire array layer, then respectively evaporating gold layers with the thickness of 50nm on two sides of the mask by a thermal evaporation method, removing the mask, and forming two unconnected gold electrodes (the distance between the two gold electrodes is 100 mu m) at the upper end of the zinc oxide nanowire array layer to obtain a complex C.
S3 sputtering to grow SiO2Decorative layer
Taking the composite obtained in the step S2 as a substrate, taking Si as a target material, controlling the sputtering temperature to be 300 ℃, the sputtering power to be 180W, the sputtering distance to be 5cm, taking the gas environment in the magnetron sputtering cavity as oxygen, the gas pressure to be 0.4Pa, sputtering for 0.5h, and forming SiO in the non-electrode area of the zinc oxide nanowire array layer2Layer (thickness 40 nm).
S4, fluorine modification treatment
The complex obtained in step S3 was suspended above an HF solution (fluorine concentration 0.01mmol/L) in which SiO was present2The layer faces to the HF solution, and the suspension height is 20 cm; heating the HF solution to 40 ℃, and treating for 10 s; and then, washing with deionized water, and drying with dry nitrogen to form the fluorine-silicon-based modification layer.
S5, fixing indium particles
And pressing and fixing indium particles (the diameter is 1mm, and the height is 0.5mm) on two independent gold electrodes respectively to obtain the ultraviolet detector.
Comparative example 1
The procedure of example 1 was followed except that no modification treatment was performed (i.e., steps S3 and S4 were not performed).
Example 2
The ultraviolet detectors obtained in example 1 and comparative example 1 were subjected to performance tests, and the results are shown in fig. 5 to 7, respectively.
FIG. 5 is a graph of I-V curves before and after modification of the UV detector. It can be seen that the dark current of the unmodified device (comparative example 1) was 66.3pA at 10V bias, and the dark current of the double modified device (example 1) was reduced to 4.5 pA.
FIG. 6 is a graph of the light response before and after modification of the UV detector. It can be seen that at 10V bias, the peak responsivity of the unmodified device (comparative example 1) is 1.0A/W, the UV suppression ratio is greater than 2 orders of magnitude; the peak responsivity of the double-modified device (example 1) is increased to 12.0A/W, and the ultraviolet suppression ratio is more than 3 orders of magnitude.
FIG. 7 is a graph of response time before and after modification of the UV detector. It can be seen that the current of the unmodified device (comparative example 1) decreased from 90% to 10% to 48ms at 10V bias, and the response time of the double modified device (example 1) decreased to 4.6 ms.
The comparison shows that the double modification of the invention can obviously reduce the dark current of the ultraviolet detector, improve the responsivity and reduce the response time.
Example 3
S1 growing zinc oxide nanowire array layer by MOCVD method
The same as in example 1.
S2 preparation of electrode
Interdigital gold electrodes (the distance between the interdigital electrodes is 5 microns, the length of an interdigital is 0.5mm, the width of the interdigital is 5 microns, the number of the interdigital electrodes in each electrode is 10, the thickness of the electrode is 50nm) are respectively prepared on two sides of a shelter through a photoetching method, two interdigital gold electrodes which are not connected with each other are formed at the upper end of a zinc oxide nanowire array layer (the distance between the two interdigital gold electrodes is 100 microns), and a complex C is obtained.
S3 sputtering to grow SiO2Decorative layer
The same as in example 1.
S4, fluorine modification treatment
The same as in example 1.
S5, fixing indium particles
The same as in example 1.
Comparative example 2
The procedure of example 3 was followed except that no modification treatment was performed (i.e., steps S3 and S4 were not performed).
Example 4
The performance tests were performed on the uv detectors obtained in example 3 and comparative example 2, respectively, and the results were as follows:
the dark current for the unmodified device (comparative example 1) was 407pA at 10V bias, and the dark current for the double modified device (example 3) was reduced to 8.9 pA.
At 10V bias, the peak responsivity of the unmodified device (comparative example 1) was 62A/W, and the UV suppression ratio was greater than 3 orders of magnitude; the peak responsivity of the double-modified device (example 3) is raised to 126A/W, and the ultraviolet suppression ratio is more than 4 orders of magnitude.
The current of the unmodified device (comparative example 1) decreased from 90% to 10% to 20ms at 10V bias, and the response time of the double modified device (example 3) decreased to 90 μ s.
The comparison shows that the double modification of the invention can obviously reduce the dark current of the ultraviolet detector, improve the responsivity and reduce the response time.
Comparative example 3
The procedure is as in example 1, except that SiO is not carried out2Modification, only the F modification was performed (i.e., step S3 was not performed).
The performance test of the obtained ultraviolet detector was carried out as in example 2, and the result showed that the dark current of the obtained device was 0.1pA, the peak responsivity was 0.01A/W, and the response time was 1500 ms. It can be seen that the performance of the device is reduced by the simple F modification. The reason is presumed to be that the overall performance of the detector is reduced because the zinc oxide nanowire array is small in size and the surface of the array film has many defects, and the zinc oxide nanowire array film material is damaged by F modification.
Examples 5 to 9
The preparation process is carried out according to the embodiment 1, except that the suspension height is changed, and the method specifically comprises the following steps: 0.1cm, 1cm, 5cm, 30cm, 50 cm.
The obtained ultraviolet detectors were subjected to performance tests according to example 2, respectively, and compared with example 1, and the results are shown in table 1.
TABLE 1 results of Performance test of examples 5 to 9
| Height in midair, cm | Dark current, pA | Responsivity, A/W | Response time, ms | |
| Example 5 | 0.1 | 0.1 | 0.1 | 1 |
| Example 6 | 1 | 0.7 | 4.8 | 2.2 |
| Example 7 | 5 | 1 | 13 | 3.2 |
| Example 1 | 20 | 4.5 | 12 | 4.6 |
| Example 8 | 30 | 40 | 7.8 | 20 |
| Example 9 | 50 | 52 | 2.7 | 33 |
As can be seen from table 1, the dark current, the responsivity and the response time of the device after double modification can be significantly improved compared to the unmodified device. Under the same condition, when the suspension height is 0.1-20 cm, dark current and response time can be further obviously reduced, and the responsiveness is further obviously improved.
Examples 10 to 14
The preparation process of example 1 was followed, except that the time of the fluorine modification treatment was changed to specifically include: 1s, 20s, 60s, 5min, 1 h.
The obtained ultraviolet detectors were subjected to performance tests according to example 2, respectively, and compared with example 1, and the results are shown in table 2.
TABLE 2 results of Performance test of examples 10 to 14
As can be seen from table 2, the dark current, the responsivity and the response time of the device after double modification of the present invention can be significantly improved compared to the unmodified device. Under the same condition, when the fluorine modification treatment time is 10-60 s, the dark current and the response time can be further obviously reduced, and the responsiveness is further obviously improved.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The zinc oxide nanowire array ultraviolet detector is characterized by comprising the following components in percentage by weight:
the device comprises a substrate and a zinc oxide nanowire array layer compounded on the surface of the substrate;
the surface of the zinc oxide nanowire array layer sequentially comprises a first electrode area, a non-electrode area and a second electrode area along the length direction;
electrodes are compounded on the first electrode area and the second electrode area; indium particles are fixed on the electrodes;
the non-electrode area is compounded with a modification layer;
the modification layer is a fluorine-silicon-based modification layer; the fluorine-silicon-based modification layer comprises: SiF4And F.
2. The ultraviolet detector according to claim 1, wherein the thickness of the zinc oxide nanowire array layer is 50-1000 nm;
the thickness of the electrode is 5-300 nm.
3. The ultraviolet detector of claim 1, wherein the electrode is a gold electrode or a gold-nickel alloy electrode.
4. The uv detector according to claim 1 or 3, characterized in that the electrodes are in the shape of bulk or interdigital electrodes.
5. The ultraviolet detector of claim 2, wherein the first electrode area is spaced from the second electrode area by 0.2-2 mm.
6. The ultraviolet detector according to claim 4, wherein the inter-finger distance of the interdigital electrodes is 1-10 μm, the interdigital length is 0.1-2 mm, the interdigital width is 1-10 μm, and the number of the interdigital electrodes in each electrode is 10-100.
7. The preparation method of the zinc oxide nanowire array ultraviolet detector as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
a) growing a zinc oxide nanowire array layer on the surface of the substrate to obtain a complex A;
b) placing a shelter in the center of the zinc oxide nanowire array layer, and sequentially dividing the surface of the zinc oxide nanowire array layer into a first electrode area, a non-electrode area and a second electrode area along the length direction; forming electrodes on the first electrode area and the second electrode area to obtain a composite body B;
c) growing SiO in the non-electrode area of the zinc oxide nanowire array layer in the compound B2Modifying the layer to obtain a composite C;
d) for SiO on the composite C2And carrying out fluorine modification treatment on the modification layer to form a fluorine-silicon-based modification layer, and fixing indium particles on the electrode to obtain the ultraviolet detector.
8. The method of claim 7, wherein the step d) comprises:
placing the compound C above a fluorine solution in the air, wherein the SiO is2The modification layer faces the fluorine solution; and heating the fluorine solution to form a fluorine-silicon-based modification layer on the zinc oxide nanowire array layer.
9. The method according to claim 7, wherein the fluorine solution is one or more of an HF solution, a KF solution, a NaF solution, a trifluoroacetic acid solution, a trifluoromethanesulfonic acid solution, and a trifluoropropionic acid solution.
10. The method according to claim 7, wherein the fluorine concentration in the fluorine solution is 1 x 10- 6mol/L～10mol/L；
The height of the suspension is 0.1-50 cm;
the temperature of the temperature rise is 25-100 ℃, and the heat preservation treatment time after the temperature rise is 0.01 s-24 h.
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