CN112993085A - Gallium oxide X-ray detector and preparation method thereof - Google Patents
Gallium oxide X-ray detector and preparation method thereof Download PDFInfo
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- CN112993085A CN112993085A CN202110176376.8A CN202110176376A CN112993085A CN 112993085 A CN112993085 A CN 112993085A CN 202110176376 A CN202110176376 A CN 202110176376A CN 112993085 A CN112993085 A CN 112993085A
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- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 142
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 138
- 239000000758 substrate Substances 0.000 claims abstract description 60
- 238000000137 annealing Methods 0.000 claims abstract description 38
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 239000010410 layer Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 239000000969 carrier Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000011241 protective layer Substances 0.000 claims description 4
- -1 air Chemical compound 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 17
- 239000003574 free electron Substances 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 229910000577 Silicon-germanium Inorganic materials 0.000 description 2
- LEVVHYCKPQWKOP-UHFFFAOYSA-N [Si].[Ge] Chemical compound [Si].[Ge] LEVVHYCKPQWKOP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 230000005284 excitation Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a gallium oxide X-ray detector and a preparation method thereof, wherein the preparation method of the gallium oxide X-ray detector comprises the following steps: providing a gallium oxide single crystal; cutting the gallium oxide single crystal to obtain a single crystal substrate sheet; annealing the single crystal substrate sheet to obtain an annealed single crystal substrate sheet; and forming an interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector. According to the invention, the gallium oxide single crystal is adopted, the gallium oxide single crystal is cut to obtain the single crystal substrate sheet, the annealing treatment is carried out on the single crystal substrate sheet, and the concentration of free electrons in the gallium oxide single crystal is reduced through the annealing treatment, so that the gallium oxide X-ray detector can respond more quickly under voltage, and the response time is shortened.
Description
Technical Field
The invention relates to the technical field of semiconductor photoelectronic devices, in particular to a gallium oxide X-ray detector and a preparation method thereof.
Background
X-ray is a high-energy ray, which has been found to have profound and widespread effects on human society, and is now widely used in the fields of medical diagnosis, environmental monitoring, security inspection, industrial nondestructive monitoring, high-grade physics, and the like. The detection of X-rays is one of the key technologies for applying X-rays, and the continuous development of materials and device technologies of X-ray detectors is an important development direction in the field of X-ray application at present. The scintillator X-ray detector is made of NaI materials commonly used, the linearity of the energy of the detected X-rays is poor, the energy resolution is poor, and the energy resolution is generally 50% -60%; and the NaI (Tl) detector needs to be provided with a photomultiplier, so that the system is heavy. The gas X-ray detector has large volume and low detection efficiency.
In the prior art, the gallium oxide X-ray detector has small volume but long response time.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a gallium oxide X-ray detector and a method for manufacturing the same, aiming at solving the problem of long response time of the gallium oxide X-ray detector in the prior art.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a method for preparing a gallium oxide X-ray detector comprises the following steps:
providing a gallium oxide single crystal;
cutting the gallium oxide single crystal to obtain a single crystal substrate sheet;
annealing the single crystal substrate sheet to obtain an annealed single crystal substrate sheet;
and forming an interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector.
The preparation method of the gallium oxide X-ray detector comprises the following steps,
the temperature of the annealing treatment is 850-1450 ℃, the time of the annealing treatment is 5-20h, and the atmosphere of the annealing treatment is oxygen or mixed gas containing oxygen.
The preparation method of the gallium oxide X-ray detector comprises the following steps,
the interdigital electrode includes: the Ti layer is connected with the annealed single crystal substrate sheet, and the conductive protective layer is connected with the Ti layer; the thickness of the Ti layer is 10-20nm, and the thickness of the conductive protection layer is 50-200 nm.
The preparation method of the gallium oxide X-ray detector comprises the following steps of: an Au layer or an Al layer; and/or the presence of a gas in the gas,
the width of an interdigital in the interdigital electrode is 50-200 μm; the interval between two adjacent fingers in the interdigital electrodes is 50-200 μm.
The preparation method of the gallium oxide X-ray detector comprises the following steps,
the method for forming the interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector comprises the following steps:
polishing and ultrasonic processing are carried out on the annealed single crystal substrate sheet to obtain an ultrasonic single crystal substrate sheet;
and forming an interdigital electrode on the ultrasonic single crystal substrate sheet by adopting magnetron sputtering coating or electron beam evaporation to obtain the gallium oxide X-ray detector.
The preparation method of the gallium oxide X-ray detector comprises the following steps,
the ultrasonic treatment adopts acetone and ethanol.
The preparation method of the gallium oxide X-ray detector comprises the following steps,
the length of the single crystal substrate sheet is 3mm-10 mm; the width of the single crystal substrate sheet is 3mm-10 mm; the thickness of the single crystal substrate sheet is 0.1mm-3 mm.
The preparation method of the gallium oxide X-ray detector comprises the step of preparing the gallium oxide single crystal by a melt method.
The preparation method of the gallium oxide X-ray detector comprises the following steps of:
drying gallium oxide powder, putting the dried gallium oxide powder into a crucible, heating and melting to obtain a gallium oxide melt, and enabling the gallium oxide melt to flow to the upper surface of a mold;
contacting seed crystals with the gallium oxide melt on the upper surface of the mold, and lifting the seed crystals to obtain the gallium oxide single crystals; or the like, or, alternatively,
the gallium oxide single crystal is prepared by adopting a floating zone method, and the specific steps are as follows:
drying gallium oxide powder, and then putting the gallium oxide powder into a crucible to be heated and melted to obtain a gallium oxide melt;
and contacting a seed crystal with the gallium oxide melt, and lifting the seed crystal to obtain the gallium oxide single crystal.
A gallium oxide X-ray detector is obtained by adopting the preparation method of the gallium oxide X-ray detector.
Has the advantages that: according to the invention, the gallium oxide single crystal is adopted, the gallium oxide single crystal is cut to obtain the single crystal substrate sheet, the annealing treatment is carried out on the single crystal substrate sheet, and the concentration of free electrons in the gallium oxide single crystal is reduced through the annealing treatment, so that the gallium oxide X-ray detector can respond more quickly under voltage, and the response time is shortened.
Drawings
FIG. 1 is a flow chart of a method of manufacturing a gallium oxide X-ray detector according to the present invention.
FIG. 2 is a cross-sectional view of a gallium oxide X-ray detector of the present invention.
FIG. 3 is a top view of a gallium oxide X-ray detector of the present invention.
FIG. 4 is a graph of the response time of a gallium oxide X-ray detector of the present invention.
FIG. 5 is a graph of the response time of a gallium oxide X-ray detector in accordance with the present invention without annealing.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1-5, the present invention provides embodiments of a method for fabricating a gallium oxide X-ray detector.
The semiconductor detector is used as an X-ray detector and has the advantages of good linear response, high energy resolution, short pulse rise time, high detection efficiency, low bias voltage, simple structure and the like. The silicon-germanium X-ray detector in the semiconductor X-ray detector has small material band gap, is sensitive to environmental temperature and has weak radiation resistance, so that the application field of the X-ray detector is limited.
As shown in fig. 1, the method for preparing a gallium oxide X-ray detector of the present invention comprises the following steps:
step S100, providing gallium oxide single crystal.
Specifically, the X-ray is electromagnetic radiation with energy between ultraviolet ray and gamma ray, and the X-ray detection technology is based on the interaction between the X-ray and a substance to generate photoconduction or ionization excitation equivalent, generate secondary electrons and generate an electric signal through back-end electronic processing. The gallium oxide X-ray detector is used as a semiconductor detector, a semiconductor material is used for absorbing high-energy X-rays and generating electron-hole pairs, and carriers induced by the X-rays are collected by an external circuit to form an electric signal. The gallium oxide single crystal is a single crystal formed by gallium oxide materials, and compared with gallium oxide polycrystal and amorphous gallium oxide, the gallium oxide single crystal is beneficial to absorption of X rays and transmission of carriers, and response time of the detector can be shortened. Gallium oxide single crystals may be prepared by a melt process comprising: floating zone methods, descent methods, heat exchange methods, pulling methods, and guided mode methods. The following description will be made by taking the die guide method and the float zone method as examples.
The gallium oxide single crystal is prepared by adopting a guide die method, and specifically, the gallium oxide single crystal is obtained by adopting the following steps:
a100, drying gallium oxide powder, putting the dried gallium oxide powder into a crucible, heating and melting to obtain a gallium oxide melt, and enabling the gallium oxide melt to flow to the upper surface of the mold.
Specifically, the gallium oxide powder may be β -gallium oxide (4N-6N) powder, and moisture in the gallium oxide powder may be removed by drying the gallium oxide powder, thereby avoiding generation of water vapor when melting the gallium oxide powder. The crucible can be an iraurita crucible, a mold is arranged in the crucible, and the mold can be an iraurita mold. After the gallium oxide is completely melted, the upper surface of the mold is higher than the surface of the gallium oxide melt in the crucible, and the gallium oxide melt in the mold lifts the gallium oxide melt in the crucible to the upper surface of the mold by utilizing capillary force.
And A200, contacting seed crystals with the gallium oxide melt on the upper surface of the mold, and lifting the seed crystals to obtain the gallium oxide single crystals.
Specifically, a seed crystal is fixed on a seed rod, and is lowered to the upper surface of a mold and is in contact with gallium oxide melt on the upper surface of the mold, and the gallium oxide single crystal is formed through three stages of necking, shouldering and stable growth.
By way of example, Ga2O3(4N-6N) powderDrying at 70 deg.C (the drying temperature can be 50-100 deg.C), placing the dried powder in iraurita crucible (with iraurita mold) surrounded by thermal insulation material, heating the iraurita crucible by electromagnetic induction heating coil to melt the gallium oxide powder, and using capillary force to heat Ga2O3The melt is transferred from the crucible to the upper surface of the mold, the seed crystal is brought into contact with the melt on the surface of the mold, and then lifted at a certain speed (about 10 mm/h). And then heating to neck, and after necking, setting a fixed cooling rate to enable the crystal to shoulder and expand in the horizontal direction, thereby starting crystal growth.
The gallium oxide single crystal is prepared by adopting a floating zone method, and specifically, the gallium oxide single crystal is obtained by adopting the following steps:
and B100, drying the gallium oxide powder to prepare a material rod, and contacting the material rod with the seed crystal.
Specifically, gallium oxide powder is subjected to cold pressing and sintering to form a material rod, the material rod is fixed on a feeding rod, a seed crystal is fixed on a seed crystal rod, and then the material rod is contacted with the seed crystal.
And B200, melting the contact position of the material rod and the seed crystal, and moving the seed crystal to obtain the gallium oxide single crystal.
Specifically, the contact position of the material rod and the seed crystal is melted, the gallium oxide of the material rod is melted and contacted with the seed crystal, and when the seed crystal is moved, a gallium oxide single crystal is formed on the seed crystal.
By way of example, beta-Ga2O3Drying (4N-6N) powder in an oven at 70 ℃, preparing the powder into a material rod, cold-pressing the material rod under 70-450 MPa and sintering the material rod at 1300-1600 ℃ to prepare the material rod with the diameter of 5-8 mm, fixing the material rod on a feeding rod, fixing seed crystals on a seed crystal rod, adjusting the rotating speed of the two rods to be 10-15 r/min, adjusting the rotating speed of the two rods to be opposite, using two halogen lamps as heat sources, focusing light to the tip of the material rod in contact with the seed crystals by using an elliptical reflector to enable the temperature of the tip to reach 1800-1900 ℃, starting melting the seed crystals, and then enabling the material rod above and the material rod below to meltThe melted seed crystal is contacted with the melt zone of the material rod and the seed crystal formed by surface tension, the melt zone is fixed at the high temperature of the lamp, and the two rods move downwards at the same speed (the moving speed is 3-5mm/h) to start to grow crystals.
And step S200, cutting the gallium oxide single crystal to obtain a single crystal substrate.
Specifically, the surface of the single crystal substrate sheet may be the 001 plane or the 100 plane of gallium oxide, and the position of the seed crystal may be arranged according to the crystal plane required for gallium oxide in the single crystal substrate sheet. The length of the single crystal substrate sheet is 3mm-10 mm; the width of the single crystal substrate sheet is 3mm-10 mm; the thickness of the single crystal substrate sheet is 0.1mm-3 mm. Since the single crystal base sheet needs to be annealed, the thickness of the single crystal base sheet is not necessarily too thick.
And step S300, annealing the single crystal substrate sheet to obtain an annealed single crystal substrate sheet.
Specifically, the temperature of the annealing treatment is 1250-1600 ℃, the time of the annealing treatment is 5-20h, and the atmosphere of the annealing treatment is air or oxygen. During the annealing, the free electron concentration of the single crystal base sheet decreases due to the generation of defects that trap electrons such as Ga vacancies; and Ga3+Electrons are captured after bond breaking, the content of low-valence Ga ions is increased, and the concentration of free electrons is reduced. In addition, annealing at high temperatures improves the quality of the single crystal of gallium oxide. The free electron concentration of the single crystal base sheet decreases more with the increase in the temperature of the annealing treatment and the extension of the time of the annealing treatment, and of course the temperature of the annealing treatment should not be too high so as not to melt the single crystal base sheet. Preferably, the temperature of the annealing treatment is 1250 ℃, and the time of the annealing treatment is 10 h. Preferably, the temperature of the annealing treatment is 1450 ℃, and the time of the annealing treatment is 20 h.
And S400, forming an interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector.
Specifically, as the annealed single crystal substrate sheet is a single crystal, the surface of the single crystal substrate sheet is a crystal surface, the interdigital electrode is formed on the crystal surface, and the crystal surface of the annealed single crystal substrate sheet is covered by a large-area interdigital electrode, as shown in fig. 3, the area of the region where the interdigital electrode is located (the area of the dashed-line frame in fig. 3) occupies an area of 1/2 or more of the annealed single crystal substrate sheet, so that the interdigital electrode can be well connected to the annealed single crystal substrate sheet, and carrier transmission is realized. And the interdigital electrode has the advantage of large area, once the annealed substrate sheet is irradiated by X rays, the generated current carriers can be immediately transferred onto the electrode, so that the response time is shortened.
Specifically, the monocrystalline substrate piece in the invention is a bulk material, the bulk material has higher crystal quality, and compared with the preparation of an X-ray detector by directly using bulk gallium oxide as a substrate, a gallium oxide photodetector epitaxially grown on the substrate (such as sapphire) has a blue shift of a band gap.
As shown in fig. 2 and 3, the interdigital electrode 20 includes: a Ti layer 21 and a conductive protective layer 22, the Ti layer 21 being connected to the annealed single crystal base sheet 10, the conductive protective layer 22 being connected to the Ti layer 21; the thickness of the Ti layer 21 is 10-20nm, and the thickness of the conductive protection layer 22 is 50-200 nm. The thickness of the Ti layer 21 is smaller than that of the conductive protection layer 22, the conductive protection layer 22 is firmly connected with gallium oxide by using the Ti layer 21, and then the conductive protection layer 22 with high carrier transmission efficiency is connected on the basis of the Ti layer 21, so that the service life of the detector is ensured. In addition, the conductive protection layer 22 may function to protect the Ti layer 21 from oxidation.
Specifically, the conductive protection layer 22 includes: the Au layer or the Al layer, that is, the Au layer electrode may be connected to the Ti layer electrode, and the Al layer electrode may be connected to the Ti layer electrode.
The width of an interdigital in the interdigital electrode is 50-200 μm; the interval between two adjacent fingers in the interdigital electrodes is 50-200 μm. The interdigital electrode 20 includes: a cathode and an anode, the cathode comprising: a first base portion to which a plurality of first fingers are connected, the anode comprising: and the plurality of first fingers and the plurality of second fingers are arranged alternately. The width of the first finger is 50 μm-200 μm, the width of the second finger is 50 μm-200 μm, and the interval between the adjacent first finger and the second finger is 50 μm-200 μm.
Specifically, step S400 includes:
and S410, polishing and ultrasonic processing are carried out on the annealed single crystal substrate sheet to obtain an ultrasonic single crystal substrate sheet.
Specifically, in order to form better connection between the electrode and the annealed single crystal substrate sheet and better absorption of X-rays, the annealed single crystal substrate sheet is subjected to polishing treatment and then ultrasonic treatment, and gallium oxide micropowder generated in the polishing treatment is removed, so that the surface of the obtained ultrasonic single crystal substrate sheet is smoother. Specifically, acetone and ethanol are adopted for ultrasonic treatment, that is, the annealed single crystal substrate sheet is polished and then put into acetone or ethanol for ultrasonic treatment, so as to obtain the ultrasonic single crystal substrate sheet.
And step S420, forming an interdigital electrode on the ultrasonic single crystal substrate sheet by adopting magnetron sputtering coating or electron beam evaporation to obtain the gallium oxide X-ray detector.
Specifically, the interdigital electrode is formed by magnetron sputtering coating or electron beam evaporation, and the electrode and the economic body can be firmly connected and the interdigital electrode can be more easily formed by magnetron sputtering coating or electron beam evaporation. For example, the parameters of magnetron sputtering coating are as follows: background vacuum degree superior to 1 × 10-4And Pa, plating Ti metal by using a direct-current power supply with the power of 200w for 30s-60s, plating Au or Al metal by using a radio-frequency power supply with the power of 120w for 60s-120 s.
The detector prepared by the invention has the following advantages:
1. the radiation-resistant characteristic of the gallium oxide X-ray detector. The Mg doping has the problems of nonuniform segregation, lattice distortion and the like. The scheme is based on intrinsic gallium oxide, has no growth difficulty caused by doping, has no newly introduced energy level defect, and has stronger radiation resistance.
2. The crystal quality is improved by annealing, the performance of the X-ray detector is improved, and the response time is shortened. Annealing is carried out in a specific oxygen-containing atmosphere, the maximum annealing temperature is 1250-1600 ℃, and the method is favorable for further reducing the carrier concentration, improving the sensitivity and shortening the response time.
3. Gallium oxide is a wide band gap semiconductor, and has a higher radiation resistance and a faster response time than the first generation silicon germanium semiconductor.
4. Compared with the preparation process, the preparation process of the interdigital electrode is simple and convenient, the dark current is small, and the response time is fast.
Detailed description of the preferred embodiment
1. 100-plane gallium oxide was grown by the guided mode method, and cut to obtain crystal pieces of 6mm × 6mm × 0.5 mm.
2. Annealing the gallium oxide substrate sheet at 1450 deg.C for 20h in air atmosphere, wherein the carrier concentration after annealing is lower than the lower limit of conventional instrument<1×1015/cm3。
3. And grinding and polishing the gallium oxide substrate sheet after the annealing is finished.
4. And after polishing, sequentially carrying out ultrasonic treatment in acetone and ethanol.
5. Ti/Au electrode (Ti layer thickness is 10 nm; Au layer electrode thickness is 50nm) interdigital electrodes are plated on the gallium oxide single crystal wafer, the width and the interval are 100 mu m, and magnetron sputtering is used for plating.
6. The response time of the device was tested by giving X-ray excitation every 30s at 1 v. The specific results are shown in FIG. 4. It can be seen that the response time of the gallium oxide X-ray detector of the present invention is 60 s.
Detailed description of the invention
In order to verify the influence of the annealing treatment on the gallium oxide X-ray detector, the gallium oxide X-ray detector without the annealing treatment is prepared, except that the annealing treatment is not performed, the steps andas with the procedure of example one, the comparison measured a carrier concentration of about 1X 10 for the unannealed sample17/cm3。
As shown in fig. 5, the response time of the non-annealed gallium oxide X-ray detector could not be determined, and was significantly longer than that of the annealed gallium oxide X-ray detector of the present invention. And the current of the gallium oxide X-ray detector annealed in the invention is less than that of the gallium oxide X-ray detector not annealed.
It should be noted that, when testing the device performance, it can also test the response time of the device before and after annealing by applying a voltage of 1-100v to the device and applying an X-ray light to it at intervals (10-30 s).
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing a gallium oxide X-ray detector is characterized by comprising the following steps:
providing a gallium oxide single crystal;
cutting the gallium oxide single crystal to obtain a single crystal substrate sheet;
annealing the single crystal substrate sheet to obtain an annealed single crystal substrate sheet;
and forming an interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector.
2. The method for producing a gallium oxide X-ray detector according to claim 1,
the temperature of the annealing treatment is 1200-1600 ℃, the time of the annealing treatment is 5-20h, the atmosphere of the annealing treatment is oxygen or mixed atmosphere containing oxygen such as air, and the concentration of carriers after annealing is carried out<1×1015/cm3。
3. The method for producing a gallium oxide X-ray detector according to claim 1,
the interdigital electrode includes: the Ti layer is connected with the annealed single crystal substrate sheet, and the conductive protective layer is connected with the Ti layer; the thickness of the Ti layer is 10-20nm, and the thickness of the conductive protection layer is 50-200 nm.
4. The method for preparing a gallium oxide X-ray detector according to claim 3, wherein the conductive protection layer comprises: an Au layer or an Al layer; and/or the presence of a gas in the gas,
the width of an interdigital in the interdigital electrode is 50-200 μm; the interval between two adjacent fingers in the interdigital electrodes is 50-200 μm.
5. The method for producing a gallium oxide X-ray detector according to claim 4,
the method for forming the interdigital electrode on the annealed single crystal substrate to obtain the gallium oxide X-ray detector comprises the following steps:
polishing and ultrasonic processing are carried out on the annealed single crystal substrate sheet to obtain an ultrasonic single crystal substrate sheet;
and forming an interdigital electrode on the ultrasonic single crystal substrate sheet by adopting magnetron sputtering coating or electron beam evaporation to obtain the gallium oxide X-ray detector.
6. The method for producing a gallium oxide X-ray detector according to claim 5,
the ultrasonic treatment adopts acetone and ethanol.
7. The method for producing a gallium oxide X-ray detector according to claim 1,
the length of the single crystal substrate sheet is 3mm-10 mm; the width of the single crystal substrate sheet is 3mm-10 mm; the thickness of the single crystal substrate sheet is 0.1mm-3 mm.
8. The method for preparing a gallium oxide X-ray detector according to claim 1, wherein the gallium oxide single crystal is prepared by a melt method.
9. The method for producing a gallium oxide X-ray detector according to claim 8,
the gallium oxide single crystal is prepared by adopting a die-guiding method, and the method comprises the following specific steps:
drying gallium oxide powder, putting the dried gallium oxide powder into a crucible, heating and melting to obtain a gallium oxide melt, and enabling the gallium oxide melt to flow to the upper surface of a mold;
contacting seed crystals with the gallium oxide melt on the upper surface of the mold, and lifting the seed crystals to obtain the gallium oxide single crystals; or the like, or, alternatively,
the gallium oxide single crystal is prepared by adopting a floating zone method, and the specific steps are as follows:
drying gallium oxide powder to prepare a material rod, and contacting the material rod with seed crystals;
and melting the contact part of the material rod and the seed crystal, and moving the seed crystal to obtain the gallium oxide single crystal.
10. A gallium oxide X-ray detector, characterized in that the gallium oxide X-ray detector is obtained by using the method for manufacturing a gallium oxide X-ray detector according to any one of claims 1 to 9.
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