CN112490318A - AlGaAs/GaAs neutron detector with PIN microstructure - Google Patents
AlGaAs/GaAs neutron detector with PIN microstructure Download PDFInfo
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Abstract
An AlGaAs/GaAs neutron detector with a PIN microstructure takes N-type GaAs as a substrate layer, and a variable doping variable component N-type AlGaAs N layer, an intrinsic GaAs I layer, a variable doping variable component P-type AlGaAs P layer and a P-type GaAs ohmic contact cap layer are sequentially grown on the GaAs substrate layer; then SiO is deposited on the p-type GaAs ohmic contact cap layer2A passivation layer, and then a variable doping variable component N-type AlGaAs N layer, an intrinsic GaAs I layer, a variable doping variable component P-type AlGaAs P layer and a P-type GaAs ohmic contact cap layer are etched in sequence to form a microstructure; forming a p-type electrode layer and an n-type electrode layer on the p-type GaAs ohmic contact cap layer and the GaAs substrate layer after the alignment; and finally, a neutron conversion layer is filled in the microstructure, so that the current carrier collection efficiency can be increased, the leakage current can be reduced, and the detection efficiency of the neutron detector can be improved.
Description
Technical Field
The invention relates to the technical field of semiconductor nuclear radiation detection, in particular to an AlGaAs/GaAs neutron detector with a PIN microstructure.
Background
The neutron detector is a core component of neutron detection. Based onThe semiconductor neutron detector has the advantages of low power consumption, wide linear response range, fast response time, good n/gamma resolution, small volume, low working voltage and the like. As a novel detection technology, in order to exert the detection performance, researchers develop related researches to prepare various GaAs nuclear radiation detectors. In 2002, McGregor et al tried to use GaAs material to fabricate a circular hole type neutron detector on a semi-insulating GaAs substrate, and the circular hole was filled with a material10B, but the highest detection efficiency of the device is only 3.9%; in 2012, the russian national academy of science prepared a GaAs schottky particle detector using an epitaxial growth method. However, the above detectors all have problems of low detection efficiency, 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 PIN microstructure to solve the above 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 PIN microstructure takes N-type GaAs as a substrate layer, and a variable doping variable component N-type AlGaAs N layer, an intrinsic GaAs I layer, a variable doping variable component P-type AlGaAs P layer and a P-type GaAs ohmic contact cap layer are sequentially grown on the GaAs substrate layer by adopting a metal organic chemical vapor deposition technology; depositing SiO on the p-type GaAs ohmic contact cap layer by using a plasma enhanced chemical vapor deposition technology2A passivation layer, and then sequentially etching the variable-doping variable-component N-type AlGaAs N layer, the intrinsic GaAs I layer, the variable-doping variable-component P-type AlGaAs P layer and the P-type GaAs ohmic contact cap layer by utilizing photoetching and dry etching technologies to form a microstructure; forming a p-type electrode layer on the p-type GaAs ohmic contact cap layer after the alignment by using an electron beam evaporation technology, forming an n-type electrode layer on the GaAs substrate layer by using the electron beam evaporation technology, and annealing the formed electrode layer to form ohmic contact; finally, filling the microstructure by utilizing ultrasonic, low-pressure condensation and centrifugation technologies10B4C or6LiF forms a neutron conversion layer.
A preparation method of an AlGaAs/GaAs neutron detector with a PIN microstructure comprises the following specific steps:
firstly, an n-type GaAs material is selected as a substrate, and the dislocation density is required to be lower than 103cm-2And has good uniformity, and the doping concentration of the n-type GaAs substrate is (0.5-2) × 1018cm-3；
Epitaxially growing a GaAs substrate layer by adopting a metal organic chemical vapor deposition technology, wherein the thickness of the epitaxial growth is 6 mu m, and the n-type doping concentration is from (0.5-5) x 1018cm-3Decreasing to (0.5-5) x 10 according to the index16cm-3The AlGaAs layer with the Al component content linearly decreasing to 0 from 0.2-0.5 is an N layer in the PIN structure;
growing intrinsic GaAs with the thickness of 1-4 mu m on the variable doping variable component N-type AlGaAs N layer to serve as an I layer in the PIN structure;
regrowing on the intrinsic GaAs I layer with a thickness of 2-18 μm and a p-type doping concentration of 0.5-5 x 1016cm-3Increasing the index to (0.5-5) x 1018cm-3The variable-band-gap AlGaAs layer with the Al component content linearly increasing from 0 to 0.2-0.5 is a P layer in the PIN structure;
growing a layer with a thickness of 50-200 nm and a doping concentration of (0.2-1) × 10 on the P-type AlGaAs P layer with variable doping and composition19cm-3The GaAs layer is used as a p-type GaAs ohmic contact cap layer;
growing a layer of SiO with the thickness of 100-800 nm on the p-type GaAs ohmic contact cap layer by utilizing a plasma enhanced chemical vapor deposition technology2A passivation layer; the reaction parameters of the reaction chamber are as follows: the pressure in the reaction chamber is 2000mTorr, and SiH is introduced4、N2O and N2The flow of the gas is 4SCCM, 710SCCM and 180SCCM respectively, the temperature of the GaAs substrate is 350 ℃, and the deposition time is 6-30 min;
by using a spin coater on SiO2Spin-coating an RPN1150 negative photoresist layer with the thickness of 1-2 μm on the passivation layer, placing the sample material coated with the negative photoresist layer into a baking machine, heating to 90-110 deg.C, baking for 100-110 s, cooling, taking out, placing into the exposure position of the photoetching machine, selecting a photoetching plate with microstructure pattern, and performing low vacuum processingExposing for 11-13 s to expose partial SiO2Simultaneously developing the passivation layer for 45-55 s by using NMD-3 developing solution, cleaning the developing solution, and drying to form a photoetching primary mask image of the neutron detector;
etching off exposed SiO on the obtained photo-etching primary mask image of the neutron detector by reactive ion etching technology2The passivation layer is used for sequentially etching an epitaxial layer by utilizing an inductive coupling plasma etching technology to form a PIN microstructure, the epitaxial layer comprises a P-type GaAs ohmic contact cap layer, a variable doping variable component P-type AlGaAs P layer, an intrinsic GaAs I layer and a variable doping variable component N-type AlGaAs N layer, and the etching structural parameters are that the width of an etched groove is 16-20 mu m, the depth is 16-20 mu m, and the distance between adjacent walls of the groove is 16-20 mu m;
ultrasonically cleaning the material containing the negative photoresist layer on the top of the PIN microstructure for 3-5 min by using acetone, ethanol and deionized water respectively to remove the negative photoresist layer;
removing the negative photoresist layer, and removing SiO contained at the top of the PIN microstructure2Removing the passivation layer, namely performing ultrasonic treatment on the passivation layer in an ultrasonic machine by using a BOE solution for 2-3 min, and performing ultrasonic treatment on the passivation layer in the ultrasonic machine by using deionized water for 3-5 min to take out the passivation layer;
removal of SiO contained on top of PIN microstructure2Performing alignment on the basis of the passivation layer, spin-coating an AZ5124 positive photoresist layer with the thickness of 1-2 mu m on the p-type GaAs ohmic contact cap layer by using a spin coater, putting the sample material coated with the positive photoresist layer into a baking machine, heating to 90-110 ℃, baking for 100-110 s, cooling, taking out, putting into an exposure position of the photoetching machine, exposing for 11-13 s in a low vacuum state, developing for 45-55 s by using NMD-3 developing solution, and drying to form a neutron detector photoetching secondary mask image;
sequentially depositing Ti/Pt/Au as ohmic contact metal on the front surface of the pattern of the obtained photoetching secondary mask image of the neutron detector by an electron beam evaporation technology to form a p-type electrode layer, 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;
heating and stripping the positive photoresist layer and the metal on the positive photoresist layer by acetone to obtain a neutron detector intermediate, wherein the heating temperature is 60-70 ℃, stripping is carried out for 18-22 min, and then the neutron detector intermediate is sequentially placed into ethanol and deionized water to be respectively subjected to ultrasonic cleaning for 3-5 min;
sequentially depositing AuGe/Ni/Au on a GaAs substrate layer on the back of an obtained neutron detector intermediate as ohmic contact metal by an electron beam evaporation technology to form an n-type electrode layer, wherein the thickness of AuGe is 80-120 nm, the thickness of Ni is 20-40 nm, and the thickness of Au is 180-220 nm; annealing the ohmic contact after metal deposition, wherein the annealing temperature is 350-450 ℃, and the annealing time is 50-70 s, so as to obtain a neutron detector converter;
filling neutron conversion layer by using a filling method combining ultrasound, low-pressure condensation and centrifugation, and firstly generating by using low-pressure condensation6LiF or10B4C nanoparticles, which will then be provided with6LiF or10B4Placing the beaker containing the C nanoparticles and the absolute ethyl alcohol into an ultrasonic cleaning machine for ultrasonic treatment to disperse the nanoparticles to form6LiF or10B4C, colloidal suspension, fixing the prepared neutron detector conversion body at the bottom of a centrifugal tube, and filling the centrifugal tube with the neutron detector conversion body subjected to ultrasonic treatment6LiF or10B4C colloidal suspension, finally rotating at high speed by a centrifuge6LiF or10B4And C, filling the colloidal suspension into a neutron detector conversion body, wherein the rotating speed of a centrifugal machine is 3500-4500 r/min, and the time is 2-3 min, so that the AlGaAs/GaAs neutron detector with the PIN microstructure is obtained.
The mechanism of the invention is as follows: AlGaAs/GaAs neutron detectors in neutron conversion layers when neutron irradiation occurs10B or6Li and neutrons generate nuclear reaction to release alpha particles, the alpha particles generate electron-hole pairs when passing through the PIN microstructure, and under the action of an electric field built in AlGaAs/GaAs and an electric field generated by an external bias, the electron-hole pairs generated in the P layer, the I layer and the N layer are effectively separated due to the fact that the electric fields are arranged in the P layer, the I layer and the N layer, so that the charge collection efficiency of carriers and the detection efficiency of a detector are improved.
Has the advantages that:
1) the neutron detector prepared by the invention adopts a microstructure, so that the contact area between a neutron conversion material and a semiconductor material can be increased, and the thermal neutron detection efficiency of the semiconductor neutron detector is greatly improved;
2) the neutron detector prepared by the invention adopts a variable doping and variable component AlGaAs/GaAs structure, so that built-in electric fields are generated in a P region and an N region, the built-in electric fields drive generated electrons and holes to respectively move towards two ends in a directional manner, the collection efficiency is effectively increased, the sensitivity and the detection efficiency of the neutron detector are improved, the magnitude of reverse bias voltage can be reduced during working, even the neutron detector can work under zero bias, and the leakage current of the neutron detector is reduced.
Drawings
FIG. 1 is a schematic diagram of a structure of an n-type GaAs substrate layer in a preferred embodiment of the present invention.
FIG. 2 is a schematic view of the structure of epitaxially grown variable-doped variable-composition N-type AlGaAs N layer in the preferred embodiment of the present invention.
FIG. 3 is a schematic view of the structure of epitaxially grown intrinsic GaAs I layer in the preferred embodiment of the present invention.
FIG. 4 is a schematic view of the structure of epitaxially grown variable-doped variable-composition P-type AlGaAs P layer in the preferred embodiment of the present invention.
FIG. 5 is a schematic diagram of a epitaxially grown p-GaAs ohmic contact cap layer structure in a preferred embodiment of the invention.
FIG. 6 is a schematic diagram of SiO deposition in a preferred embodiment of the invention2And the passivation layer structure is shown schematically.
FIG. 7 is a schematic view of a structure of a negative photoresist layer spun on in a preferred embodiment of the invention.
FIG. 8 is a schematic diagram of a photolithographic one-time mask image structure of a neutron detector in a preferred embodiment of the invention.
FIG. 9 is a schematic diagram of etching away exposed SiO portions in a preferred embodiment of the invention2And the passivation layer structure is shown schematically.
Fig. 10 is a schematic diagram illustrating a structure after etching the epitaxial layer according to the preferred embodiment of the invention.
FIG. 11 is a schematic view of the structure after the removal of the negative photoresist layer in the preferred embodiment of the invention.
FIG. 12 is a schematic diagram of SiO removal in a preferred embodiment of the invention2And the post-passivation structure is schematically shown.
FIG. 13 is a schematic diagram of a lithographic secondary mask image structure of a neutron detector in a preferred embodiment of the invention.
FIG. 14 is a schematic view of a structure of depositing a p-type electrode layer in a preferred embodiment of the invention.
FIG. 15 is a schematic view of a structure for stripping a positive photoresist layer in a preferred embodiment of the invention.
FIG. 16 is a schematic view of a structure of depositing an n-type electrode layer in a preferred embodiment of the invention.
Fig. 17 is a schematic view of a filled neutron conversion layer 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 preparation method of an AlGaAs/GaAs neutron detector with a PIN groove structure comprises the following specific steps:
as shown in FIG. 1, first, n-type doping concentration of 1X 10 is 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-2；
As shown in FIG. 2, a GaAs substrate layer 1 is epitaxially grown by MOCVD to a thickness of 6 μm and an n-type doping concentration of 1 × 1018cm-3Decreasing exponentially to 1 × 1016cm-3The AlGaAs layer with the Al component content linearly decreasing from 0.4 to 0 is an N layer 2 in the PIN structure;
as shown in fig. 3, intrinsic GaAs with a thickness of 2 μm is grown as an I layer 3 on a variable-doping variable-composition N-type AlGaAs N layer 2;
as shown in FIG. 4, a 10 μm thick intrinsic GaAs I layer 3 was regrown with a p-type doping concentration of 1X 1016cm-3Exponentially increasing to 5X 1018cm-3The variable-band-gap AlGaAs layer with the Al component content linearly increasing from 0 to 0.4 is a P layer 4 in the PIN structure;
as shown in FIG. 5, a layer of 100nm thick doped 5X 10 doped P-type AlGaAs P layer 4 is grown on the substrate18cm-3The GaAs layer is used as a p-type GaAs ohmic contact cap layer 5;
as shown in FIG. 6, a layer of SiO with a thickness of 100nm is grown on the p-type GaAs ohmic contact cap layer 5 by using the plasma enhanced chemical vapor deposition technique2 A passivation layer 6;
as shown in FIG. 7, a spin coater was used to coat SiO2Spin-coating a layer of RPN1150 negative photoresist layer 7 with thickness of 1.5 μm on the passivation layer 6, placing the sample material coated with the negative photoresist layer 7 in a baking machine, heating to 100 deg.C, baking for 100s, cooling, taking out, placing in the exposure position of the photoetching machine, selecting a photoetching plate with groove structure pattern, exposing for 12s in low vacuum state to expose partial SiO2A passivation layer 6, simultaneously developing for 50s by using NMD-3 developing solution, cleaning the developing solution, and drying to form a photoetching primary mask image containing the neutron detector shown in the figure 8;
as shown in FIG. 9, the exposed portion of SiO is etched away by reactive ion etching technique on the acquired photo-etching primary mask image of the neutron detector2A passivation layer 6, sequentially etching an epitaxial layer by using an inductive coupling plasma etching technology to form a PIN groove structure, wherein the epitaxial layer comprises a P-type GaAs ohmic contact cap layer 5, a variable doping variable component P-type AlGaAs P layer 4, an intrinsic GaAs I layer 3 and a variable doping variable component N-type AlGaAs N layer 2, the etching structure parameters are that the width of the etching groove is 18 mu m, the depth of the etching groove is 18 mu m, the distance between adjacent walls of the groove is 18 mu m, and the etching groove is taken out as shown in figure 10 after etching;
as shown in fig. 11, the material containing the negative photoresist layer 7 on the top of the PIN trench structure is ultrasonically cleaned for 3min by acetone, ethanol and deionized water respectively to remove the negative photoresist layer 7;
as shown in fig. 12, on the basis of removing the negative photoresist layer 7, the SiO contained on the top of the PIN trench structure2Removing the passivation layer 6, and carrying out ultrasonication in an ultrasonic machine by using BOE solutionSounding for 2min, and then ultrasonically treating in an ultrasonic machine for 3min by using deionized water;
as shown in fig. 13, the SiO contained on the top of the removed PIN trench structure2Performing alignment on the passivation layer 6, spin-coating an AZ5124 positive photoresist layer 8 with the thickness of 1.5 mu m on the p-type GaAs ohmic contact cap layer 5 by using a spin coater, putting the sample material coated with the positive photoresist layer 8 into a baking machine, heating to 100 ℃, baking for 100s, cooling, taking out, putting into an exposure position of the photoetching machine, exposing for 12s in a low vacuum state, developing for 50s by using NMD-3 developing solution, and drying to form a photoetching secondary mask image containing the neutron detector shown in FIG. 13;
as shown in fig. 14, by an electron beam evaporation technique, Ti/Pt/Au as an ohmic contact metal was sequentially deposited on the pattern front surface of the obtained neutron detector lithography secondary mask image to form a p-type electrode layer 9, wherein Ti was 50nm thick, Pt was 50nm thick, and Au was 200nm thick;
as shown in fig. 15, the positive photoresist layer 8 and the metal thereon are heated and stripped by acetone to obtain a neutron detector intermediate, the heating temperature is 60 ℃, stripping is performed for 20min, and then the neutron detector intermediate is sequentially placed into ethanol and deionized water to be ultrasonically cleaned for 3min respectively;
as shown in fig. 16, sequentially depositing AuGe/Ni/Au as ohmic contact metal on the GaAs substrate layer 1 on the back of the obtained neutron detector intermediate by an electron beam evaporation technique to form an n-type electrode layer 10, wherein the thickness of AuGe is 100nm, the thickness of Ni is 35nm, and the thickness of Au is 200 nm; annealing the ohmic contact after metal deposition, wherein the annealing temperature is 400 ℃, and the annealing time is 60s, so as to obtain a neutron detector converter;
as shown in FIG. 17, neutron conversion layer filling was performed by weighing 0.1g by a filling method combining ultrasound and centrifugation6Pouring LiF powder and 8ml of absolute ethyl alcohol into a beaker, and then putting the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5min so as to disperse particles to form6LiF colloidal suspension, fixing the prepared neutron detector converter at the bottom of a centrifugal tube, and filling the centrifugal tube with the ultrasonically treated neutron detector converter6A colloidal suspension of LiF in water, in the form of a suspension,and finally, filling the nano-particle powder into a micro-groove of a neutron detector conversion body through high-speed rotation of a centrifugal machine, wherein the rotating speed of the centrifugal machine is 4000r/min, and the time is 2min, so that the AlGaAs/GaAs neutron detector with the PIN groove structure is obtained.
Example 2
A preparation method of a PIN columnar structure AlGaAs/GaAs neutron detector comprises the following specific steps:
as shown in FIG. 1, first, n-type doping concentration of 1X 10 is 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-2；
As shown in FIG. 2, a GaAs substrate layer 1 is epitaxially grown by MOCVD to a thickness of 8 μm and an n-type doping concentration of 1 × 1018cm-3Decreasing exponentially to 1 × 1016cm-3The AlGaAs layer with the Al component content linearly decreasing from 0.4 to 0 is an N layer 2 in the PIN structure;
as shown in fig. 3, intrinsic GaAs with a thickness of 3 μm is grown as an I layer 3 on a variable-doping variable-composition N-type AlGaAs N layer 2;
as shown in FIG. 4, the intrinsic GaAs I layer 3 was grown to a thickness of 14 μm with a p-type doping concentration of 1X 1016cm-3Exponentially increasing to 5X 1018cm-3The variable-band-gap AlGaAs layer with the Al component content linearly increasing from 0 to 0.4 is a P layer 4 in the PIN structure;
as shown in FIG. 5, a layer of 100nm thick doped 5X 10 doped P-type AlGaAs P layer 4 is grown on the substrate18cm-3The GaAs layer is used as a p-type GaAs ohmic contact cap layer 5;
as shown in FIG. 6, a layer of SiO with a thickness of 100nm is grown on the p-type GaAs ohmic contact cap layer 5 by using the plasma enhanced chemical vapor deposition technique2 A passivation layer 6;
as shown in FIG. 7, a spin coater was used to coat SiO2Spin-coating a layer of RPN1150 negative photoresist layer 7 with a thickness of 1.5 μm on the passivation layer 6, placing the sample material coated with the negative photoresist layer 7 into a baking machine, heating to 100 deg.C, baking for 100s, cooling, taking out, and placing in a lightExposing the lithography machine with a cylindrical photolithography plate under low vacuum for 12s to expose partial SiO2 A passivation layer 6, simultaneously developing for 50s by using NMD-3 developing solution, cleaning the developing solution, and drying to form a photoetching primary mask image containing the neutron detector shown in the figure 8;
as shown in FIG. 9, the exposed portion of SiO is etched away by reactive ion etching technique on the acquired photo-etching primary mask image of the neutron detector2 A passivation layer 6, and sequentially etching the P-type GaAs ohmic contact cap layer 5, the variable doping variable component P-type AlGaAs P layer 4, the intrinsic GaAs I layer 3 and the variable doping variable component N-type AlGaAs N layer 2 by utilizing an inductive coupling plasma etching technology to form a PIN columnar structure, wherein the etching structure has the parameters that the diameter of a column is 20 mu m, the height of the column is 25 mu m, the distance between adjacent walls of the column is 20 mu m, and the column is taken out as shown in the figure 10 after etching;
as shown in fig. 11, the material containing the negative photoresist layer 7 on the top of the PIN columnar structure is ultrasonically cleaned for 3min by acetone, ethanol and deionized water respectively to remove the negative photoresist layer 7;
as shown in fig. 12, on the basis of removing the negative photoresist layer 7, the SiO contained on the top of the PIN columnar structure2Removing the passivation layer 6, performing ultrasonic treatment in an ultrasonic machine for 2min by adopting BOE solution, and performing ultrasonic treatment in the ultrasonic machine for 3min by using deionized water to take out;
as shown in FIG. 13, SiO contained at the top of the removed PIN pillar structure2Performing alignment on the passivation layer 6, spin-coating an AZ5124 positive photoresist layer 8 with the thickness of 1.5 mu m on the p-type GaAs ohmic contact cap layer 5 by using a spin coater, putting the sample material coated with the positive photoresist layer 8 into a baking machine, heating to 100 ℃, baking for 100s, cooling, taking out, putting into an exposure position of the photoetching machine, exposing for 12s in a low vacuum state, developing for 50s by using NMD-3 developing solution, and drying to form a photoetching secondary mask image containing the neutron detector shown in FIG. 13;
as shown in fig. 14, by an electron beam evaporation technique, Ti/Pt/Au as an ohmic contact metal was sequentially deposited on the pattern front surface of the obtained neutron detector lithography secondary mask image to form a p-type electrode layer 9, wherein Ti was 50nm thick, Pt was 50nm thick, and Au was 200nm thick;
as shown in fig. 15, the positive photoresist layer 8 and the metal thereon are heated and stripped by acetone to obtain a neutron detector intermediate, the heating temperature is 60 ℃, and stripping is carried out for 20 min;
as shown in fig. 16, sequentially depositing AuGe/Ni/Au as ohmic contact metal on the GaAs substrate layer 1 on the back of the obtained neutron detector intermediate by an electron beam evaporation technique to form an n-type electrode layer 10, wherein the thickness of AuGe is 100nm, the thickness of Ni is 35nm, and the thickness of Au is 200 nm; annealing the ohmic contact after metal deposition, wherein the annealing temperature is 400 ℃, and the annealing time is 60s, so that a neutron detector conversion cylinder is obtained;
as shown in FIG. 17, the neutron conversion layer was filled by a filling method combining ultrasound and centrifugation, in which 0.1g was first weighed6Pouring LiF powder and 8ml of absolute ethyl alcohol into a beaker, and then putting the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5min so as to disperse particles to form6LiF colloidal suspension, fixing the prepared neutron detector conversion body at the bottom of a centrifugal tube, and filling the centrifugal tube with the ultrasonically treated neutron detector conversion body6And (3) filling the nano-particle powder into a column structure of a neutron detector conversion column through high-speed rotation of a centrifugal machine, wherein the rotating speed of the centrifugal machine is 4000r/min, and the time is 2min, so that the AlGaAs/GaAs neutron detector with the PIN columnar structure is obtained.
Example 3
A preparation method of an AlGaAs/GaAs neutron detector with a PIN hole type structure comprises the following specific steps:
as shown in FIG. 1, first, n-type doping concentration of 1X 10 is 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-2；
As shown in FIG. 2, a GaAs substrate layer 1 is epitaxially grown by MOCVD to a thickness of 3 μm and an n-type doping concentration of 1 × 1018cm-3Decreasing exponentially to 1 × 1016cm-3The AlGaAs layer in which the Al component content linearly decreases from 0.4 to 0 is PINAn N layer 2 in the structure;
as shown in fig. 3, GaAs is grown as an I layer 3 with a thickness of 1 μm on a variable-doping variable-composition N-type AlGaAs N layer 2;
as shown in FIG. 4, a 5 μm thick intrinsic GaAs I layer 3 was regrown with a p-type doping concentration of 1X 1016cm-3Exponentially increasing to 5X 1018cm-3The variable-band-gap AlGaAs layer with the Al component content linearly increasing from 0 to 0.4 is a P layer 4 in the PIN structure;
as shown in FIG. 5, a layer of 100nm thick doped 5X 10 doped P-type AlGaAs P layer 4 is grown on the substrate18cm-3The GaAs layer is used as a p-type GaAs ohmic contact cap layer 5;
as shown in FIG. 6, a layer of SiO with a thickness of 100nm is grown on the p-type GaAs ohmic contact cap layer 5 by using the plasma enhanced chemical vapor deposition technique2Passivating layer 6, setting the pressure of reaction chamber to 2000mTorr, and introducing SiH4、N2O and N2The flow of the gas is 4SCCM, 710SCCM and 180SCCM respectively, and the substrate temperature is 350 ℃;
as shown in FIG. 7, a spin coater was used to coat SiO2Spin-coating a layer of RPN1150 negative photoresist layer 7 with thickness of 1.5 μm on the passivation layer 6, placing the sample material coated with the negative photoresist layer 7 into a baking machine, heating to 100 deg.C, baking for 100s, cooling, taking out, placing into the exposure position of the photoetching machine, exposing for 12s under low vacuum condition with a photoetching plate having hole-shaped structure pattern to expose partial SiO2 A passivation layer 6, simultaneously developing for 50s by using NMD-3 developing solution, cleaning the developing solution, and drying to form a photoetching primary mask image containing the neutron detector shown in the figure 8;
as shown in FIG. 9, the exposed portion of SiO is etched away by reactive ion etching technique on the acquired photo-etching primary mask image of the neutron detector2And a passivation layer 6, sequentially etching the P-type GaAs ohmic contact cap layer 5, the variable-doping variable-component P-type AlGaAs P layer 4, the intrinsic GaAs I layer 3 and the variable-doping variable-component N-type AlGaAs N layer 2 by using an inductive coupling plasma etching technology to form a PIN hole type structure, wherein the etching structure parameters are as follows: the diameter of the hole is 15 μm, the depth of the hole is 9 μm, the distance between the adjacent walls of the hole is 15 μm, and the hole is taken out after etchingAs shown in FIG. 10;
as shown in fig. 11, the material containing the negative photoresist layer 7 on the top of the PIN hole type structure is ultrasonically cleaned for 3min by acetone, isopropanol and deionized water respectively to remove the negative photoresist layer 7;
as shown in fig. 12, on the basis of removing the negative photoresist layer 7, the SiO contained on top of the PIN hole type structure2Removing the passivation layer 6, performing ultrasonic treatment in an ultrasonic machine for 2min by adopting BOE solution, and performing ultrasonic treatment in the ultrasonic machine for 3min by using deionized water to take out;
as shown in FIG. 13, SiO contained at the top of the removed PIN hole type structure2Performing alignment on the passivation layer 6, spin-coating an AZ5124 positive photoresist layer 8 with the thickness of 1.5 mu m on the p-type GaAs ohmic contact cap layer 5 by using a spin coater, putting the sample material coated with the positive photoresist layer 8 into a baking machine, heating to 100 ℃, baking for 100s, cooling, taking out, putting into an exposure position of the photoetching machine, exposing for 12s in a low vacuum state, developing for 50s by using NMD-3 developing solution, and drying to form a photoetching secondary mask image containing the neutron detector shown in FIG. 13;
as shown in fig. 14, by an electron beam evaporation technique, Ti/Pt/Au as an ohmic contact metal was sequentially deposited on the pattern front surface of the obtained neutron detector lithography secondary mask image to form a p-type electrode layer 9, wherein Ti was 50nm thick, Pt was 50nm thick, and Au was 200nm thick;
as shown in fig. 15, the positive photoresist layer 8 and the metal thereon are heated and stripped by acetone to obtain a neutron detector intermediate, the heating temperature is 60 ℃, and stripping is carried out for 20 min;
as shown in fig. 16, sequentially depositing AuGe/Ni/Au as ohmic contact metal on the GaAs substrate layer 1 on the back of the obtained neutron detector intermediate by an electron beam evaporation technique to form an n-type electrode layer 10, wherein the thickness of AuGe is 100nm, the thickness of Ni is 35nm, and the thickness of Au is 200 nm; annealing the ohmic contact after metal deposition, wherein the annealing temperature is 400 ℃, and the annealing time is 60s, so as to obtain a conversion hole body of the neutron detector;
as shown in FIG. 17, neutron conversion layer filling is performed by combining ultrasound and centrifugationFilling method, first weighing 0.1g10B4Pouring the C powder and 8ml of absolute ethyl alcohol into a beaker, and then putting the beaker into an ultrasonic cleaning machine for 5min to disperse particles to form6LiF colloidal suspension, fixing the prepared neutron detector conversion hole body at the bottom of a centrifugal tube, and filling the centrifugal tube with the processed neutron detector conversion hole body6And (3) filling the nano-particle powder into a round hole of a neutron detector conversion hole body through high-speed rotation of a centrifugal machine, wherein the rotating speed of the centrifugal machine is 4000r/min, and the time is 2min, so that the AlGaAs/GaAs neutron detector with the PIN hole type structure is obtained.
Claims (10)
1. An AlGaAs/GaAs neutron detector with a PIN microstructure is characterized in that N-type GaAs is used as a substrate layer, and a variable doping variable component N-type AlGaAs N layer, an intrinsic GaAs I layer, a variable doping variable component P-type AlGaAs P layer and a P-type GaAs ohmic contact cap layer are sequentially grown on the GaAs substrate layer; then SiO is deposited on the p-type GaAs ohmic contact cap layer2Passivating the layer, and then forming a microstructure in the variable-doping variable-component N-type AlGaAs N layer, the intrinsic GaAs I layer, the variable-doping variable-component P-type AlGaAs P layer and the P-type GaAs ohmic contact cap layer by utilizing dry etching; forming a p-type electrode layer on the p-type GaAs ohmic contact cap layer after the alignment, and forming an n-type electrode layer on the GaAs substrate layer; and finally, filling a neutron conversion material in the microstructure by utilizing ultrasound, low-pressure condensation and centrifugation to form a neutron conversion layer.
2. The AlGaAs/GaAs neutron detector of claim 1, wherein the etched microstructure is a trench structure, a pillar structure or a circular hole structure.
3. The AlGaAs/GaAs neutron detector with the PIN microstructure according to claim 2, wherein a width of a groove in the groove structure is 5-30 μm, a distance between adjacent walls of the groove is 5-30 μm, and a depth of the groove is 5-30 μm; in the columnar structure, the diameter of a cylinder is 5-30 mu m, the height of the column is 5-30 mu m, and the distance between adjacent walls of the column is 5-30 mu m; in the circular hole structure, the diameter of the circular hole is 5-30 mu m, the depth of the circular hole is 5-30 mu m, and the distance between adjacent walls of the circular hole is 5-30 mu m.
4. The AlGaAs/GaAs neutron detector with the PIN microstructure according to claim 1, wherein the p-type electrode layer uses Ti/Pt/Au as an ohmic contact metal, 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.
5. The AlGaAs/GaAs neutron detector with the PIN microstructure according to claim 1, wherein the n-type electrode layer adopts AuGe/Ni/Au as ohmic contact metal, wherein the AuGe is 80-120 nm thick, the Ni is 20-40 nm thick, and the Au is 180-220 nm thick.
6. The AlGaAs/GaAs neutron detector with PIN microstructure according to claim 1, wherein a neutron conversion material in the neutron conversion layer is10B4C or6LiF。
7. The method for preparing an AlGaAs/GaAs neutron detector with a PIN microstructure according to claim 1, which comprises the following steps:
firstly, preparing an n-type doped GaAs substrate base material as a GaAs substrate layer;
epitaxially growing a variable doping variable component N-type AlGaAs N layer on the GaAs substrate layer by adopting a metal organic chemical vapor deposition technology;
growing an intrinsic GaAs I layer on the variable-doping variable-component N-type AlGaAs N layer;
growing a variable doping variable component P-type AlGaAs P layer on the intrinsic GaAs I layer;
growing a P-type GaAs ohmic contact cap layer on the variable doping variable component P-type AlGaAs P layer;
growing SiO on p-type GaAs ohmic contact cap layer by utilizing plasma enhanced chemical vapor deposition technology2A passivation layer;
by using a spin coater on SiO2Spin-coating a negative photoresist layer on the passivation layer, baking the sample material coated with the negative photoresist layer in a baking machine, cooling, taking out, placing in an exposure position of the photoetching machine, selecting a photoetching plate with a microstructure pattern, and exposing in a low vacuum state to expose partial SiO2A passivation layer, developing by using NMD-3 developing solution, cleaning the developing solution, and drying to form a neutron detector photoetching primary mask image;
etching off exposed SiO on the obtained photo-etching primary mask image of the neutron detector by reactive ion etching technology2Sequentially etching an epitaxial layer comprising a P-type GaAs ohmic contact cap layer, a variable doping variable component P-type AlGaAs P layer, an intrinsic GaAs I layer and a variable doping variable component N-type AlGaAs N layer by utilizing an inductive coupling plasma etching technology to form a PIN microstructure;
removing the negative photoresist layer contained at the top of the PIN microstructure;
removing the negative photoresist layer, and removing SiO contained at the top of the PIN microstructure2Removing the passivation layer;
removal of SiO contained on top of PIN microstructure2Carrying out alignment on the basis of the passivation layer, carrying out spin coating of a positive photoresist layer on the p-type GaAs ohmic contact cap layer by using a spin coater, putting a sample material coated with the positive photoresist layer into a baking machine, heating, baking, cooling, taking out, putting into an exposure position of the photoetching machine, carrying out exposure in a low vacuum state, developing by using NMD-3 developing solution, and drying to form a neutron detector photoetching secondary mask image;
sequentially depositing Ti/Pt/Au as ohmic contact metal on the front surface of the pattern of the obtained photoetching secondary mask image of the neutron detector by an electron beam evaporation technology to form a p-type electrode layer;
heating and stripping the positive photoresist layer and the metal on the positive photoresist layer by acetone to obtain a neutron detector intermediate;
sequentially depositing AuGe/Ni/Au on the GaAs substrate layer on the back of the obtained neutron detector intermediate as ohmic contact metal by an electron beam evaporation technology to form an n-type electrode layer; annealing the ohmic contact after metal deposition to obtain a neutron detector converter;
and finally, filling a neutron conversion layer, and filling a neutron conversion material in the microstructure to form the neutron conversion layer by adopting a filling method combining ultrasound, low-pressure condensation and centrifugation to obtain the AlGaAs/GaAs neutron detector with the PIN microstructure.
8. The method for preparing an AlGaAs/GaAs neutron detector with a PIN microstructure according to claim 7, wherein the photolithography plate with a microstructure pattern comprises a photolithography plate with a groove structure pattern, a photolithography plate with a column structure pattern and a photolithography plate with a hole structure pattern.
9. The method for preparing an AlGaAs/GaAs neutron detector with a PIN microstructure according to claim 7, wherein an annealing temperature is 350-450 ℃ and an annealing time is 50-70 s in the annealing treatment.
10. The method for preparing AlGaAs/GaAs neutron detector with PIN microstructure according to claim 7, wherein the neutron conversion layer filling comprises the following steps:
produced by low-pressure condensation6LiF or10B4C nanoparticles, which will then be provided with6LiF or10B4Placing the beaker containing the C nanoparticles and the absolute ethyl alcohol into an ultrasonic cleaning machine for ultrasonic treatment to disperse the nanoparticles to form6LiF or10B4C, colloidal suspension, fixing the prepared neutron detector conversion body at the bottom of a centrifugal tube, and filling the centrifugal tube with the neutron detector conversion body subjected to ultrasonic treatment6LiF or10B4C colloidal suspension, finally rotating at high speed by a centrifuge6LiF or10B4And C, filling the colloidal suspension into the neutron detector converter.
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