CN112490319A - AlGaAs/GaAs neutron detector with micro-groove by wet etching - Google Patents

AlGaAs/GaAs neutron detector with micro-groove by wet etching Download PDF

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CN112490319A
CN112490319A CN202011353730.1A CN202011353730A CN112490319A CN 112490319 A CN112490319 A CN 112490319A CN 202011353730 A CN202011353730 A CN 202011353730A CN 112490319 A CN112490319 A CN 112490319A
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gaas
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CN112490319B (en
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汤彬
邹继军
陈大洪
彭新村
朱志甫
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East China Institute of Technology
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Abstract

An AlGaAs/GaAs neutron detector with a micro-groove etched by a wet method uses p-type GaAs as a substrate layer, a low Al component variable band gap AlGaAs/GaAs active layer and a high Al component AlGaAs etching layer are sequentially epitaxially grown on the GaAs substrate layer, then a plurality of layers of low Al component variable band gap AlGaAs/GaAs active layers and high Al component AlGaAs etching layers are periodically and alternately grown on the high Al component AlGaAs etching layer, finally, the layer epitaxially grown on the top layer is the low Al component variable band gap AlGaAs/GaAs active layer, and then the high Al component AlGaAs etching layer is etched by HF acid to form the micro-groove; and a Schottky electrode is deposited in the micro-groove, an ohmic electrode is deposited on the GaAs substrate layer, and finally a neutron conversion layer is formed in the micro-groove, so that the etched micro-groove has obvious quality, and the neutron detection efficiency of the detector is improved.

Description

AlGaAs/GaAs neutron detector with micro-groove by wet etching
Technical Field
The invention relates to the technical field of semiconductor nuclear radiation detection, in particular to an AlGaAs/GaAs neutron detector with a micro-groove etched by a wet method.
Background
Neutrons are not charged themselves and cannot lose energy by ionization, excitation, and so on. Therefore, the conventional semiconductor neutron detector is realized by depositing a neutron conversion layer on the surface of a semiconductor device, but the detection efficiency and the energy resolution of the semiconductor neutron detector are low due to the problems of low neutron absorption rate, self-absorption of reaction products and the like. GaAs is an important III-V group compound semiconductor material, has the advantages of radiation resistance, high electron mobility, high response speed and the like, and foreign scholars conduct deep research on the GaAs material in order to improve the detection efficiency of a semiconductor neutron detector. In 2000, Vernon et al developed10The high-purity epitaxial GaAs thermal neutron detector of the coating B, the thickness range of the active layer of the detector is between 1 mu m and 5 mu m, and the detection efficiency is between 1.6 percent and 2.6 percent; in 2002, McGregor et al, Cansasii university, USA, fabricated a circular hole type neutron detector on a semi-insulating GaAs substrate by dry etching, the circular hole was filled with a material10B, but the highest detection efficiency of the device was only 3.9% measured. The detector has the problems of large leakage current and low carrier collection efficiency to a certain extent.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide an AlGaAs/GaAs neutron detector with micro-trenches by wet etching, so as to solve the above-mentioned problems in the background art.
The technical problem solved by the invention is realized by adopting the following technical scheme:
an AlGaAs/GaAs neutron detector with a micro groove etched by a wet method uses p-type GaAs as a substrate layer, a low Al component variable band gap AlGaAs/GaAs active layer and a high Al component AlGaAs etching layer are epitaxially grown on the GaAs substrate layer in sequence by adopting a metal organic chemical vapor deposition technology, then a plurality of layers of low Al component variable band gap AlGaAs/GaAs active layers and high Al component AlGaAs etching layers are periodically and alternately grown on the high Al component AlGaAs etching layer, finally, one layer epitaxially grown on the top layer is the low Al component variable band gap AlGaAs/GaAs active layer, then the high Al component AlGaAs etching layers on two side edges are corroded by HF acid, and the low Al component variable band gap AlGaAs/GaAs active layer and the high Al component AlGaAs etching layer positioned in the middle part are reserved to form the micro groove; and depositing a Schottky electrode in the micro-groove, depositing an ohmic electrode on the GaAs substrate layer, and finally filling the neutron conversion material into the micro-groove by a hanging drop rolling method to form the neutron conversion layer.
A method for manufacturing an AlGaAs/GaAs neutron detector with a micro-groove by wet etching comprises the following specific steps:
first, a p-type dopant concentration of (0.5-2). times.10 is prepared18cm-3The GaAs substrate base material is used as a GaAs substrate layer, the substrate has good uniformity and the dislocation density is lower than 103cm-2；
Epitaxially growing p-type doping concentration of 1 × 10 on GaAs substrate layer by adopting metal organic chemical vapor deposition technology18cm-3When the low Al component variable band gap AlGaAs/GaAs active layer grows outwards from the GaAs substrate layer, the Al component of the active layer increases from 0 to 0.2-0.35 in a linear mode, and then decreases from 0.2-0.35 in a linear mode to 0, and the thickness of the active layer is 4-6 mu m;
epitaxially growing p-type doping concentration of 1 × 10 on low Al composition variable band gap AlGaAs/GaAs active layer18cm-3The high Al component AlGaAs etching layer has an Al component of 0.65-0.8 and a thickness of 3-8 μm;
periodically and alternately growing 4-8 layers of low Al component variable band gap AlGaAs/GaAs active layers and high Al component AlGaAs etching layers on the high Al component AlGaAs etching layer, and finally epitaxially growing one layer of low Al component variable band gap AlGaAs/GaAs active layer on the top layer to obtain a variable band gap AlGaAs/GaAs epitaxial wafer;
scribing the grown variable-band-gap AlGaAs/GaAs epitaxial wafer to form a 2mm multiplied by 10mm strip-shaped sample, sequentially putting the strip-shaped sample into acetone alcohol deionized water for ultrasonic cleaning for 10min, drying the strip-shaped sample by blowing with nitrogen, and corroding the high Al component AlGaAs etching layer in HF acid with the concentration of 40% to form a micro-groove, wherein the corrosion time is 40-120 min, and the corrosion temperature is 25-30 ℃;
depositing Al metal on the front surface of the micro-groove by using a thermal resistance evaporation coating method to serve as a Schottky electrode, wherein the thickness of Al is 200-300 nm, and sequentially depositing Ti/Pt/Au metal on the back surface of the GaAs substrate layer by using an electron beam evaporation coating method to serve as an ohmic contact electrode, wherein the thickness of Ti is 40-60 nm, the thickness of Pt is 50nm, and the thickness of Au is 180-220 nm; annealing treatment is carried out after metal deposition, the annealing temperature is 350-450 ℃, the annealing time is 50-70 s, and a neutron detector conversion body is obtained;
finally, filling a neutron conversion layer, pouring acetic acid, hydrogen peroxide and a methanol solution into a beaker according to the volume ratio of 1:1:1, mixing to obtain a mixed solution, and slowly pouring the mixed solution into the beaker10B4C or6In LiF powder, the mixed solution can be used as a lubricant to reduce the friction between particles and between the particles and the side wall of the groove, and then the mixture is placed into an ultrasonic cleaning machine for 5min to disperse the particles to form10B4C or6Suspending drop of LiF colloid, fixing the neutron detector converter on the fixture along the long edge direction, keeping the fixture surface and the neutron detector converter surface parallel and level, and adding the suspension drop10B4C or6LiF colloid is suspended on the surface of the high Al component AlGaAs etching layer of the neutron detector conversion body, and is repeatedly promoted by the surface of the high Al component AlGaAs etching layer by using a soft foam ink roller10B4C or6And (3) enabling LiF colloid hanging drops to enter the micro-grooves, filling the back of the neutron detector conversion body in the same way, and finally, putting the filled neutron detector conversion body in a drying box for drying to finally manufacture the AlGaAs/GaAs neutron detector with the micro-grooves.
The mechanism of the invention is as follows: when incident neutrons are irradiated on the micro-groove nuclear radiation neutron detector, the incident thermal neutrons will be in contact with10B4C or6And (3) LiF reaction, generating secondary particles or rays, entering an adjacent variable-bandgap active region to form energy deposition, generating free carriers in the energy deposition process, generating electrode drift under the action of a built-in electric field, and collecting the electrode drift, thereby realizing high-efficiency nuclear radiation detection.
Has the advantages that:
1) the invention effectively solves the problem of wet etching of GaAs-based materials by utilizing the selective wet etching characteristics of AlGaAs and GaAs, the quality of the micro-groove etched by the wet method is obviously superior to that etched by the dry method, and the improvement of the neutron detection efficiency of the detector is facilitated;
2) the neutron detector prepared by the invention adopts a variable-band-gap AlGaAs/GaAs structure, the variable-band-gap AlGaAs/GaAs structure forms a built-in electric field in an energy band, so that charge carriers generated under the action of neutrons drift towards an electrode of the neutron detector nearby under the action of the built-in electric field, and the defect of high intrinsic impurity concentration of a GaAs-based material is overcome.
Drawings
FIG. 1 is a schematic diagram of a p-type GaAs substrate layer according to a preferred embodiment of the present invention.
FIG. 2 is a schematic diagram of the structure of epitaxially grown low Al composition variable bandgap AlGaAs/GaAs active layer in a preferred embodiment of the present invention.
FIG. 3 is a schematic diagram of the structure of epitaxially grown AlGaAs etched layers with high Al composition in accordance with the preferred embodiment of the present invention.
FIG. 4 is a schematic diagram of the periodic alternate growth of low Al composition variable bandgap AlGaAs/GaAs active layer and high Al composition AlGaAs etch layer structure in the preferred embodiment of the present invention.
FIG. 5 is a schematic diagram of the top epitaxially grown low Al composition bandgap AlGaAs/GaAs active layer structure in the preferred embodiment of the present invention.
FIG. 6 is a schematic diagram of a wet etching micro-trench structure in accordance with a preferred embodiment of the present invention.
Fig. 7 is a schematic diagram illustrating the fabrication of a schottky electrode according to a preferred embodiment of the present invention.
FIG. 8 is a schematic diagram of ohmic electrode preparation in a preferred embodiment of the invention.
Fig. 9 is a schematic view of a neutron conversion layer filling structure in a preferred embodiment of the invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
Example 1
A method for manufacturing an AlGaAs/GaAs neutron detector with a micro-groove by wet etching comprises the following specific steps:
first, a p-type dopant concentration of 1X 10 was prepared18cm-3The GaAs substrate base material is used as a GaAs substrate layer 1, the substrate has good uniformity and the dislocation density is lower than 103cm-2As shown in fig. 1;
epitaxially growing p-type doping concentration of 1 × 10 on GaAs substrate layer 1 by adopting metal organic chemical vapor deposition technology18cm-3When the low Al composition variable bandgap AlGaAs/GaAs active layer 2 grows outwards from the GaAs substrate layer 1, the Al composition of the active layer 2 increases linearly from 0 to 0.25 and then decreases linearly from 0.25 to 0, and the thickness of the active layer 2 is 4 μm, as shown in FIG. 2;
as shown in FIG. 3, a p-type dopant concentration of 1X 10 is epitaxially grown on the low Al composition variable bandgap AlGaAs/GaAs active layer 218cm-3The high Al component AlGaAs etching layer 3, the Al component is 0.7, and the thickness is 4 μm;
as shown in fig. 4, 5 layers of low Al composition bandgap-changed AlGaAs/GaAs active layer 2 and high Al composition AlGaAs etching layer 3 are periodically and alternately grown, and finally, one layer of low Al composition bandgap-changed AlGaAs/GaAs active layer 2 is epitaxially grown on the top layer, so as to obtain a bandgap-changed AlGaAs/GaAs epitaxial wafer, as shown in fig. 5;
as shown in fig. 6, a grown variable band gap AlGaAs/GaAs epitaxial wafer is diced to form a 2mm × 10mm strip sample, then the strip sample is sequentially placed in acetone alcohol deionized water for ultrasonic cleaning for 10min, and then nitrogen is blown dry to corrode the high Al component AlGaAs etching layer 3 in HF acid with the concentration of 40% to form a micro-groove 4, wherein the corrosion time is 60min, and the corrosion temperature is 26 ℃;
as shown in fig. 7, depositing Al metal on the front surface of the micro-trench 4 by a thermal resistance evaporation coating method to form a schottky electrode 5, wherein the thickness of Al is 200nm, and depositing Ti/Pt/Au metal on the back surface of the GaAs substrate layer 1 by an electron beam evaporation coating method to form an ohmic contact electrode 6, wherein the thickness of Ti is 50nm, the thickness of Pt is 50nm, and the thickness of Au is 200 nm; annealing treatment is carried out after metal deposition, the annealing temperature is 400 ℃, the annealing time is 60s, and a neutron detector conversion body is obtained, as shown in fig. 8;
finally, filling the neutron conversion layer 7, respectively measuring 3ml of acetic acid, hydrogen peroxide and methanol solution by adopting a hanging drop rolling method, pouring into a beaker to be mixed to obtain a mixed solution, and slowly pouring 0.1g of the mixed solution into the beaker10B4C powder, then putting into an ultrasonic cleaning machine for 5min to disperse particles to form10B4C, suspending drop of colloid, fixing the neutron detector converter on the fixture along the long edge direction, keeping the fixture surface and the neutron detector converter surface at the same level, and then adding the colloid to the fixture10B4C colloid is suspended on the surface of the high Al component AlGaAs etching layer 3 of the neutron detector conversion body, and is repeatedly promoted by the surface of the high Al component AlGaAs etching layer 3 by using a soft foam ink roller10B4C colloidal hanging drop is put into the micro-groove 4 to fill the back of the neutron detector conversion body in the same way, wherein the ink roller rolls for 200 times on each side and is rewound after every 50 times10B4C colloid is dripped on the surface of the AlGaAs etching layer 3 with high Al component in a hanging mode, finally, the filled neutron detector conversion body is placed in a drying oven to be dried, the temperature of the drying oven is set to be 100 ℃, the drying time is 30min, and finally the AlGaAs/GaAs neutron detector with the micro-grooves is manufactured as shown in figure 9.
Example 2
A method for manufacturing an AlGaAs/GaAs neutron detector with a micro-groove by wet etching comprises the following specific steps:
first, a p-type dopant concentration of 5X 10 was prepared17cm-3The GaAs substrate base material is used as a GaAs substrate layer 1, the substrate has good uniformity and the dislocation density is lower than 103cm-2As shown in fig. 1;
epitaxially growing p-type doping concentration of 5 × 10 on GaAs substrate layer 1 by adopting metal organic chemical vapor deposition technology17cm-3The Al component of the active layer 2 linearly increases from 0 when growing outwards from the GaAs substrate layer 1Increasing to 0.3 and then linearly decreasing from 0.3 to 0, the thickness of the active layer 2 is 6 μm, as shown in fig. 2;
as shown in FIG. 3, a p-type dopant concentration of 5X 10 is epitaxially grown on the low Al composition variable bandgap AlGaAs/GaAs active layer 217cm-3The high Al component AlGaAs etching layer 3 has an Al component of 0.75 and a thickness of 6 mu m;
as shown in fig. 4, 4 layers of low Al composition bandgap-changed AlGaAs/GaAs active layer 2 and high Al composition AlGaAs etching layer 3 are alternately grown periodically, and finally, one layer epitaxially grown on the top layer is the low Al composition bandgap-changed AlGaAs/GaAs active layer 2; a variable bandgap AlGaAs/GaAs epitaxial wafer as shown in FIG. 5;
as shown in fig. 6, a grown variable band gap AlGaAs/GaAs epitaxial wafer is diced to form a 2mm × 10mm strip sample, then the strip sample is sequentially placed in acetone alcohol deionized water for ultrasonic cleaning for 10min, and then nitrogen is blown dry to corrode the high Al component AlGaAs etching layer 3 in HF acid with the mass percentage concentration of 40% to form a micro-groove 4, wherein the corrosion time is 100min, and the corrosion temperature is 26 ℃;
as shown in fig. 7, depositing Al metal in the front micro-trench 4 by using a thermal resistance evaporation coating method as a schottky electrode 5, wherein the thickness of Al is 300nm, depositing Ti metal on the back of the GaAs substrate layer 1 by using an electron beam evaporation coating method, and then sequentially depositing Pt/Au by using the thermal resistance evaporation coating method as an ohmic contact electrode 6, wherein the thickness of Ti is 50nm, the thickness of Pt is 50nm, the thickness of Au is 200nm, performing annealing treatment after depositing the metal, wherein the annealing temperature is 420 ℃, and the annealing time is 60s, thereby obtaining a neutron detector converter, as shown in fig. 8;
finally, filling the neutron conversion layer 7, respectively measuring 3ml of acetic acid, hydrogen peroxide and methanol solution by adopting a hanging drop rolling method, pouring the solution into a beaker to be mixed to obtain a mixed solution, and slowly pouring the mixed solution into 0.1g of the beaker6Adding LiF powder into the solution, and then putting the solution into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5min to disperse particles to form6LiF colloidal suspension, fixing the neutron detector converter on a fixture along the long edge direction, keeping the fixture surface and the neutron detector converter surface parallel and level, and then fixing the neutron detector converter on the fixture surface6LiF glueThe bulk suspension is suspended on the surface of the high Al component AlGaAs etch layer 3 and repeatedly forced through the surface of the high Al component AlGaAs etch layer 3 using a soft foam ink roller6The LiF colloidal suspension enters the microgrooves 4 and fills the back of the neutron detector converter in the same way, wherein the ink roller rolls 160 times on each side and will be replaced after every 40 times6And (3) hanging and dropping the LiF colloidal suspension on the surface of the AlGaAs etching layer 3 with the high Al component, and finally, putting the filled neutron detector conversion body into a drying oven for drying, wherein the temperature of the drying oven is set to be 110 ℃, and the drying time is 30min, so that the AlGaAs/GaAs neutron detector with the micro-grooves is finally manufactured as shown in FIG. 9.

Claims (10)

1. An AlGaAs/GaAs neutron detector with a micro-groove etched by a wet method is characterized in that p-type GaAs is used as a substrate layer, a low Al component variable band gap AlGaAs/GaAs active layer and a high Al component AlGaAs etching layer are epitaxially grown on the GaAs substrate layer in sequence, then a plurality of layers of low Al component variable band gap AlGaAs/GaAs active layers and high Al component AlGaAs etching layers are periodically and alternately grown on the high Al component AlGaAs etching layer, finally, one layer epitaxially grown on the top layer is the low Al component variable band gap AlGaAs/GaAs active layer, then two sides of the high Al component AlGaAs etching layer are corroded by HF acid, and the low Al component variable band gap AlGaAs/GaAs active layer and the high Al component AlGaAs etching layer positioned in the middle are reserved to form the micro-groove; and depositing a Schottky electrode in the micro-groove, depositing an ohmic electrode on the GaAs substrate layer, and finally filling the neutron conversion material into the micro-groove by a hanging drop rolling method to form the neutron conversion layer.
2. The AlGaAs/GaAs neutron detector with micro-grooves formed by wet etching as claimed in claim 1, wherein 4-8 low Al composition variable bandgap AlGaAs/GaAs active layers and high Al composition AlGaAs etching layers are periodically and alternately grown on the high Al composition AlGaAs etching layer.
3. The AlGaAs/GaAs neutron detector with micro-grooves by wet etching as claimed in claim 1, whereinThe neutron conversion material is10B4C or6LiF。
4. The AlGaAs/GaAs neutron detector with the micro-groove etched by the wet method as recited in claim 1, wherein Al metal is deposited on the front surface of the micro-groove by a thermal resistance evaporation coating method to be used as a Schottky electrode, and the thickness of Al is 200-300 nm; and sequentially depositing Ti/Pt/Au metal as an ohmic contact electrode on the back of the GaAs substrate layer by adopting an electron beam evaporation coating method.
5. The AlGaAs/GaAs neutron detector with micro-grooves etched by a wet method according to claim 4, wherein the thickness of Ti is 40-60 nm, the thickness of Pt is 40-60 nm, and the thickness of Au is 180-220 nm.
6. The method for manufacturing the AlGaAs/GaAs neutron detector with the micro-grooves by wet etching according to claim 1 is characterized by comprising the following steps of:
firstly, preparing a p-type doped GaAs substrate base material as a GaAs substrate layer;
epitaxially growing a p-type doped low Al component variable band gap AlGaAs/GaAs active layer on the GaAs substrate layer by adopting a metal organic chemical vapor deposition technology;
epitaxially growing a p-type doped AlGaAs etching layer with high Al component on the AlGaAs/GaAs active layer with the variable band gap with low Al component;
periodically and alternately growing a plurality of layers of low Al component variable band gap AlGaAs/GaAs active layers and high Al component AlGaAs etching layers on the high Al component AlGaAs etching layer, and finally epitaxially growing a layer of low Al component variable band gap AlGaAs/GaAs active layer on the top layer to obtain a variable band gap AlGaAs/GaAs epitaxial wafer;
scribing the grown variable band gap AlGaAs/GaAs epitaxial wafer to form a strip-shaped sample, sequentially putting the strip-shaped sample into acetone alcohol deionized water for ultrasonic treatment for 10min for organic cleaning, blow-drying by nitrogen, and then putting into HF acid for corroding the AlGaAs etching layer with the high Al component to form a micro-groove;
depositing Al metal on the front surface of the micro-groove by using a thermal resistance evaporation coating method to serve as a Schottky electrode, wherein the thickness of Al is 200-300 nm, and sequentially depositing Ti/Pt/Au metal on the back surface of the GaAs substrate layer by using an electron beam evaporation coating method to serve as an ohmic contact electrode, wherein the thickness of Ti is 40-60 nm, the thickness of Pt is 50nm, and the thickness of Au is 180-220 nm; annealing treatment is carried out after metal deposition to obtain a neutron detector conversion body;
finally, filling a neutron conversion layer, pouring acetic acid, hydrogen peroxide and a methanol solution into a beaker according to the volume ratio of 1:1:1, mixing to obtain a mixed solution, and slowly pouring the mixed solution into the beaker10B4C or6Adding LiF powder into the solution, and then putting the solution into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5min to disperse particles to form10B4C or6Suspending drop of LiF colloid, fixing the neutron detector converter on the fixture along the long edge direction, keeping the fixture surface and the neutron detector converter surface parallel and level, and adding the suspension drop10B4C or6Suspending LiF colloid on the surface of the high Al component AlGaAs etching layer of the neutron detector converter, and repeatedly passing through the surface of the high Al component AlGaAs etching layer by using an ink roller to promote10B4C or6And (3) enabling LiF colloid hanging drops to enter the micro-grooves, filling the back of the neutron detector conversion body in the same way, and finally, putting the filled neutron detector conversion body in a drying box for drying to finally manufacture the AlGaAs/GaAs neutron detector with the micro-grooves.
7. The method as claimed in claim 6, wherein the Al composition of the active layer increases linearly from 0 to 0.2-0.35 and decreases linearly from 0.2-0.35 to 0 when growing outwards from the GaAs substrate layer, and the thickness of the active layer is 4-6 μm.
8. The method for preparing AlGaAs/GaAs neutron detector with micro-grooves by wet etching as claimed in claim 6, wherein the HF acid concentration is 40% by mass.
9. The method for preparing an AlGaAs/GaAs neutron detector with micro-grooves by wet etching according to claim 6, wherein the etching time is 40-120 min, and the etching temperature is 25-30 ℃.
10. The method for preparing an AlGaAs/GaAs neutron detector with micro-grooves by wet etching according to claim 6, wherein the annealing temperature of the annealing treatment is 350-450 ℃ and the annealing time is 50-70 s.
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