CN110335907B - MgZnO/ZnO solar blind detector with vertical structure - Google Patents
MgZnO/ZnO solar blind detector with vertical structure Download PDFInfo
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- 239000000758 substrate Substances 0.000 claims abstract description 45
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims description 32
- 238000001514 detection method Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
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- 238000004381 surface treatment Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 239000007772 electrode material Substances 0.000 claims description 6
- 238000000206 photolithography Methods 0.000 claims description 6
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
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- 238000010438 heat treatment Methods 0.000 claims 1
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- 230000008021 deposition Effects 0.000 description 27
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- 239000011777 magnesium Substances 0.000 description 10
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- 238000013112 stability test Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
- H01L31/02966—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe including ternary compounds, e.g. HgCdTe
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- H01L31/1832—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe comprising ternary compounds, e.g. Hg Cd Te
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Abstract
The invention relates to the related technical field of solar blind detectors, and particularly provides a vertical MgZnO/ZnO heterojunction solar blind detector with ZnO single crystal as a conductive substrate and a preparation method thereof. The first aspect of the invention provides a hexagonal phase solar blind band gap MgZnO film, which is prepared from Mg serving as a raw materialxZnyO，x+y＝1,0.25≤x≤0.45，0.75≤y≤0.55。
Description
Technical Field
The invention relates to the related technical field of solar blind detectors, and particularly provides a vertical MgZnO/ZnO heterojunction solar blind detector with ZnO single crystal as a conductive substrate and a preparation method thereof.
Background
The solar blind detection can obtain a high signal-to-noise ratio, and is widely applied to the fields of missile early warning, fire alarm, high-voltage corona monitoring, ozone cavity monitoring, ultraviolet local communication and the like. The traditional photoelectric vacuum detection device mainly uses mature photomultiplier as a core technology, but the traditional photoelectric vacuum detection device has huge volume, high working voltage and high cost. The solid detection device is based on semiconductor materials and has the characteristics of miniaturization, low voltage, easy integration and the like. Silicon-based semiconductor detectors are the most mature at present, but have low intrinsic quantum efficiency of ultraviolet light and need heavy filtering devices. Therefore, a solar blind detector which realizes high intrinsic quantum efficiency and wavelength selection by using the wide-bandgap semi-material becomes a research hotspot.
The MgZnO system has wide adjustable band gap, good chemical stability and radiation resistance, and can realize ultrahigh ultraviolet gain and responsivity. Therefore, MgZnO-based detectors are expected to achieve high performance in the solar-blind ultraviolet band. However, due to lattice adaptation, the MgZnO system has the problem of structural phase separation under high Mg content, and the detection performance of the MgZnO system in solar blind detection is limited. There is a need to provide a detector with better responsiveness.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a hexagonal phase solar-blind band gap MgZnO thin film, which is prepared from Mg as a raw materialxZnyO，x+y＝1,0.25≤x≤0.45，0.75≤y≤0.55。
As a preferred technical scheme of the invention, the MgZnO film with the hexagonal phase solar blind band gap is prepared by adopting a pulse laser deposition method, the laser wavelength is 248nm, and the pulse energy is 180-220 mJ.
The invention provides a vertical detection device containing the MgZnO film with the hexagonal phase solar-blind band gap.
In a preferred embodiment of the present invention, the electrode material is a ZnO single crystal substrate.
The invention also comprises a Ti/Au electrode.
As a preferred technical scheme of the invention, the thickness of the Ti electrode is 15-25 nm, and the thickness of the Au electrode is 90-110 nm.
The third aspect of the invention provides a preparation method of the vertical detection device, which comprises the steps of substrate pretreatment, substrate preheating, deposition, cooling, photoetching, evaporation and photoresist removal.
As a preferred technical solution of the present invention, the substrate pretreatment process includes sequentially cleaning a ZnO substrate with acetone, ethanol, and deionized water, and then performing surface treatment under oxygen plasma.
As a preferred technical solution of the present invention, wherein the photolithography process is photolithography of the half-interdigital electrode; wherein the finger pitch is 3-5 μm, the finger width is 3-5 μm, and the finger thickness is 230-270 μm.
The fourth aspect of the invention provides the application of the vertical detection device for fire alarm, ozone cavity detection and arc detection of an ultra-high voltage power transmission system.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains" or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the stated range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", etc., i.e., the ranges subsumed before and after the "-" as the minimum and maximum values, respectively. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range. The various embodiments, examples or illustrations described in this specification, as well as features of the various embodiments, examples or illustrations, may be combined and combined by those skilled in the art without contradiction.
In the description herein, reference to the description of the term "one preferred embodiment," "some preferred embodiments," "as a preferred aspect," "an example" or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the example or example is included in at least one example or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
First of the inventionThe aspect provides a hexagonal phase solar blind band gap MgZnO film, and the preparation raw material is MgxZnyO, x + y is 1, x is more than or equal to 0.25 and less than or equal to 0.45, and y is more than or equal to 0.75 and less than or equal to 0.55; there may be mentioned: mg (magnesium)0.3Zn0.7O、Mg0.43Zn0.57O, and the like.
In one embodiment, when the starting material is Mg0.43Zn0.57O, the band gap is 4.43eV, the single hexagonal phase is presented, the diffraction peak of the (002) surface is 34.72 degrees, the line width of the twinned swing curve is 226arcsec, the lattice constant of the c axis is 0.516nm, and the lattice mismatch is 0.8 percent.
In one embodiment, the MgZnO film with the hexagonal phase solar blind band gap is prepared by adopting a pulse laser deposition method.
The invention provides a vertical detection device containing the MgZnO film with the hexagonal phase solar-blind band gap.
In one embodiment, the vertical detection device uses a ZnO single crystal substrate as an electrode material.
In one embodiment, the vertical probing device further comprises a Ti/Au electrode; preferably, the thickness of the Ti electrode is 15-25 nm, and the thickness of the Au electrode is 90-110 nm; more preferably, the Ti electrode thickness is 20nm and the Au electrode thickness is 100 nm.
The third aspect of the invention provides a preparation method of the vertical detection device, which comprises the steps of substrate pretreatment, substrate preheating, deposition, cooling, photoetching, evaporation and photoresist removal; preferably, the method for manufacturing the vertical detection device sequentially comprises the steps of substrate pretreatment, substrate preheating, deposition, cooling, photoetching, evaporation and photoresist removal.
In one embodiment, the substrate pretreatment process comprises the steps of sequentially cleaning a ZnO substrate with acetone, ethanol and deionized water, and then carrying out surface treatment under oxygen plasma; preferably, the substrate pretreatment process comprises the steps of sequentially cleaning the ZnO substrate for 5-15 min by using acetone, ethanol and deionized water, and then carrying out surface treatment for 10-30 s under oxygen plasma; more preferably, the substrate pretreatment process is to sequentially clean the ZnO substrate with acetone, ethanol and deionized water for 10min, and then perform surface treatment under oxygen plasma for 20 s.
In one embodiment, the substrate preheating process is: 4.50X 10 in the deposition chamber-8～5.5×10-8Raising the temperature to 600-800 ℃ section by section under the Torr vacuum degree until the vacuum degree of the deposition chamber returns to 10 again-6Torr or less as a standard; after desorption, the oxygen pressure was adjusted to the deposition oxygen pressure (1.5X 10)-2～1.0×10-2Torr) and cooling to 500-600 ℃; preferably, 5.0 × 10 in the deposition chamber-8The temperature is increased to 700 ℃ section by section under the vacuum degree of the Torr until the vacuum degree of the deposition chamber is returned to 10 again-6Torr or less as a standard; after desorption, the oxygen pressure was adjusted to the deposition oxygen pressure (1.2X 10)-2Torr), and the temperature is reduced to 550 ℃.
In one embodiment, the laser wavelength is 248nm and the pulse energy is 180-220 mJ during the deposition process; preferably, the laser wavelength during deposition is 248nm and the pulse energy is 200 mJ.
In one embodiment, the pulse length during deposition is 15-25 nm, and the pulse frequency is 3-7 Hz; preferably, the pulse length during deposition is 20nm and the pulse frequency is 5 Hz.
In one embodiment, the area of the laser spot focused during the deposition process is 3-4.5 mm2And may be exemplified as 3.1mm2，3.2mm2，3.3mm2，3.4mm2，3.5mm2，3.6mm2，3.7mm2，3.8mm2，3.9mm2，4.0mm2，4.1mm2，4.2mm2，4.3mm2，4.4mm2，4.5mm2And the like.
In one embodiment, the effective energy density during deposition is 4-5.5J cm-2Examples of such a method include: 4.1J cm-2，4.2J cm-2，4.3J cm-2，4.4J cm-2，4.5J cm-2，4.6J cm-2，4.7J cm-2，4.8J cm-2，4.9J cm-2，5.0J cm-2，5.1J cm-2，5.2J cm-2，5.3J cm-2，5.4J cm-2，5.5J cm-2And the like.
In one embodiment, the number of pulses during the deposition process is 30000 to 35000; preferably, the number of pulses during deposition is 32000.
In one embodiment, the distance between the substrate targets is 60-100 mm; preferably, the liner target distance is 80 mm.
In one embodiment, the temperature is reduced to room temperature at 3-7K/min; preferably, the temperature reduction process is to reduce the temperature to room temperature at 5K/min.
In one embodiment, the photolithography process is photolithography of the half-interdigitated electrodes; wherein the finger spacing is 3-5 μm, the finger width is 3-5 μm, and the interdigital thickness is 230-270 μm; preferably, the finger pitch is 4 μm, the finger width is 4 μm, and the finger thickness is 250 μm.
In one embodiment, the photo-receiving area in the photolithography process is (180-220) × (220-270) [ mu ] m2(ii) a Preferably, the light receiving area in the photoetching process is 200X 250 μm2。
In one embodiment, the photoresist is removed using acetone.
Example 1
Embodiment 1 of the present invention provides a vertical detection device, which uses a ZnO single crystal substrate as an electrode material thereof, and further includes a Ti/Au electrode, the Ti electrode having a thickness of 20nm and the Au electrode having a thickness of 100 nm;
the preparation method of the vertical detector sequentially comprises the steps of substrate pretreatment, substrate preheating and Mg application0.3Zn0.7O deposition, cooling, photoetching, evaporation and removing the photoresist by using acetone;
the pretreatment process of the substrate comprises the steps of sequentially cleaning a ZnO substrate for 10min by using acetone, ethanol and deionized water, and then carrying out surface treatment for 20s under oxygen plasma;
the substrate preheating process comprises the following steps: 5.0 x 10 in the deposition chamber-8The temperature is increased to 700 ℃ section by section under the vacuum degree of the Torr until the vacuum degree of the deposition chamber is returned to 10 again-6Torr or less as a standard; after desorption, the oxygen pressure was adjusted to the deposition oxygen pressure (1.2X 10)- 2Torr), and reducing the temperature to 550 ℃;
the laser wavelength is 248nm and the pulse energy is in the deposition process200mJ, pulse length of 20nm, pulse frequency of 5Hz, and laser spot focusing area of 4mm2Effective energy density of 5J cm-2The number of pulses is 32000, and the distance between the lining targets is 80 mm;
the temperature reduction process is to reduce the temperature to room temperature at 5K/min;
the photoetching process is to photoetch half interdigital electrode, the finger space is 4 μm, the finger width is 4 μm, the interdigital thickness is 250 μm, and the light receiving area is 200 × 250 μm2。
Example 2
Embodiment 2 of the present invention provides a vertical detection device, which uses a ZnO single crystal substrate as an electrode material thereof, and further includes a Ti/Au electrode, the Ti electrode having a thickness of 25nm, the Au electrode having a thickness of 110 nm;
the preparation method of the vertical detection device sequentially comprises the steps of substrate pretreatment, substrate preheating and Mg application0.3Zn0.7O deposition, cooling, photoetching, evaporation and removing the photoresist by using acetone;
the substrate pretreatment process comprises the steps of sequentially cleaning a ZnO substrate for 15min by using acetone, ethanol and deionized water, and then carrying out surface treatment for 30s under oxygen plasma;
the preheating process of the substrate comprises the following steps: 5.5X 10 in the deposition chamber-8Raising the temperature to 800 ℃ section by section under the vacuum degree of Torr until the vacuum degree of the deposition chamber returns to 10 again-6Torr or less as a standard; after desorption, the oxygen pressure was adjusted to the deposition oxygen pressure (1.5X 10)- 2Torr), cooling to 600 ℃;
in the deposition process, the laser wavelength is 248nm, the pulse energy is 220mJ, the pulse length is 25nm, the pulse frequency is 7Hz, and the area of laser spot focusing is 4.5mm2Effective energy density of 5.5J cm-2The number of pulses is 35000, and the distance of the lining target is 100 mm;
the temperature reduction process is to reduce the temperature to room temperature at 7K/min;
the photoetching process is to photoetch half interdigital electrodes, the finger distance is 5 μm, the finger width is 5 μm, the interdigital thickness is 270 μm, and the light receiving area is 220 × 270 μm2。
Example 3
Embodiment 3 of the present invention provides a vertical detection device, which uses a ZnO single crystal substrate as an electrode material thereof, and further includes a Ti/Au electrode, the Ti electrode having a thickness of 15nm, the Au electrode having a thickness of 90 nm;
the preparation method of the vertical detection device sequentially comprises the steps of substrate pretreatment, substrate preheating and Mg application0.3Zn0.7O deposition, cooling, photoetching, evaporation and removing the photoresist by using acetone;
the substrate pretreatment process comprises the steps of sequentially cleaning a ZnO substrate for 5min by using acetone, ethanol and deionized water, and then carrying out surface treatment for 10s under oxygen plasma;
the substrate preheating process comprises the following steps: in the deposition chamber 4.5X 10-8Raising the temperature to 600 ℃ section by section under the vacuum degree of the Torr until the vacuum degree of the deposition chamber returns to 10 again-6Torr or less as a standard; after desorption, the oxygen pressure was adjusted to the deposition oxygen pressure (1.0X 10)- 2Torr) and cooling to 500 ℃;
the laser wavelength is 248nm, the pulse energy is 180mJ, the pulse length is 15nm, the pulse frequency is 3Hz, and the area of laser spot focusing is 3mm in the deposition process2Effective energy density of 4J cm-2The number of pulses is 30000, and the distance between the lining targets is 60 mm;
the temperature reduction process is to reduce the temperature to room temperature at 3K/min;
the photoetching process is to photoetch half interdigital electrode, the finger space is 3 μm, the finger width is 3 μm, the interdigital thickness is 230 μm, and the light receiving area is 180X 220 μm2。
Example 4
Example 4 of the present invention provides a vertical probe device, which is similar to example 1 except that Mg is used0.49Zn0.51And depositing O.
Example 5
Embodiment 5 of the present invention provides a vertical detection device, which is similar to embodiment 1 in the specific implementation manner, except that the Ti electrode has a thickness of 10nm and the Au electrode has a thickness of 80 nm.
Example 6
Embodiment 6 of the present invention provides a vertical detection device, which is similar to embodiment 1 in the specific implementation manner, except that the thickness of the Ti electrode is 35nm, and the thickness of the Au electrode is 120 nm.
Example 7
Embodiment 7 of the present invention provides a vertical probing device, which is similar to embodiment 1 in that the finger pitch is 8 μm, the finger width is 8 μm, and the finger thickness is 300 μm.
Example 8
An embodiment 8 of the present invention provides a vertical probing device, which is similar to the embodiment 1, but has a finger pitch of 4 μm, a finger width of 4 μm, and an interdigital thickness of 200 μm.
Performance evaluation:
1. and (3) photoelectric response test: photoelectric response tests are carried out on the test systems in the embodiments 1-3 described in the table 1, and the experimental results are shown in the table 4;
2. photoelectric response spectrum test: the test system described in Table 2 is adopted to carry out photoelectric response spectrum test on the embodiments 1-3, and the experimental result is as follows: under 5V bias, the response peak of examples 1 to 3 is 278nm according to e-1The cut-off wavelength of the reduction is 286nm, and the inhibition ratio at 350nm is more than 6000;
3. and (3) testing photoelectric response stability: the test system described in Table 3 is adopted to carry out the photoelectric response stability test on the embodiments 1-8, namely, whether the response degree is maintained at 2A/W within 100 cycles under the 5V bias is observed to have obvious attenuation or not, and the experimental result is shown in Table 4.
Table 1 test system configuration table
TABLE 2 test system configuration Table
TABLE 3 test system configuration Table
TABLE 4 photoelectric response test results
The MgZnO film with the high-quality hexagonal phase solar-blind band gap on the ZnO single crystal substrate has the characteristics of single hexagonal phase, good lattice quality, solar-blind band gap and substrate conduction, and improves the responsivity and stability of a detector.
Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (4)
1. A vertical detector of an MgZnO film with a hexagonal phase solar-blind band gap is characterized in that the MgZnO film with the hexagonal phase solar-blind band gap is prepared from MgxZnyO as a raw material, wherein x + y =1, x is more than or equal to 0.25 and less than or equal to 0.45, and y is more than or equal to 0.75 and less than or equal to 0.55;
the electrode material of the vertical detection device is a ZnO single crystal substrate;
the vertical detection device also comprises a Ti/Au electrode;
the thickness of the Ti electrode is 15-25 nm, and the thickness of the Au electrode is 90-110 nm;
the electrodes are photoetching semi-interdigital electrodes; wherein the finger spacing is 3-5 μm, the finger width is 3-5 μm, and the finger length is 230-270 μm;
the MgZnO film with the hexagonal phase solar blind band gap is prepared by a pulse laser deposition method, the laser wavelength is 248nm, and the pulse energy is 180-220 mJ.
2. The method for manufacturing a vertical probing device according to claim 1, comprising the steps of pre-treating the substrate, pre-heating the substrate, depositing, cooling, photolithography, evaporating and removing the photoresist.
3. The method for manufacturing a vertical probing device according to claim 2, wherein the substrate pre-treatment comprises sequentially cleaning the ZnO substrate with acetone, ethanol and deionized water, and performing surface treatment under oxygen plasma.
4. The vertical detection device according to any one of claims 1 to 3, which is used for fire alarm, ozone hole detection and arc detection in an ultra-high voltage power transmission system.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910646981.XA CN110335907B (en) | 2019-07-17 | 2019-07-17 | MgZnO/ZnO solar blind detector with vertical structure |
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| CN201910646981.XA CN110335907B (en) | 2019-07-17 | 2019-07-17 | MgZnO/ZnO solar blind detector with vertical structure |
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| CN110335907A CN110335907A (en) | 2019-10-15 |
| CN110335907B true CN110335907B (en) | 2022-07-12 |
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| WO2002001650A1 (en) * | 2000-06-26 | 2002-01-03 | University Of Maryland | Mgzno based uv detectors |
| CN102031487A (en) * | 2010-10-11 | 2011-04-27 | 深圳大学 | Hexagonal MgZnO film with high magnesium content and preparation method thereof |
| US9059417B1 (en) * | 2013-06-06 | 2015-06-16 | University Of Central Florida Research Foundation, Inc. | Photodetectors based on wurtzite MgZnO |
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| Lower temperature growth of single phase MgZnO films in all Mg content range;Xu Wang等;《Journal of Alloys and Compounds》;20141230;第627卷;第383页右栏第1段-386页右栏第3段 * |
| MgZnO-based metal-semiconductor-metal solar-blind photodetectors on ZnO substrates;Qinghong Zheng等;《Applied Physics Letters》;20110603;第98卷;第221112.1-3页 * |
| Qinghong Zheng等.MgZnO-based metal-semiconductor-metal solar-blind photodetectors on ZnO substrates.《Applied Physics Letters》.2011,第98卷第221112.1-3页. * |
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