CN103094405A - Preparation process of CdZnTe detector of capacitive Frisch grid - Google Patents
Preparation process of CdZnTe detector of capacitive Frisch grid Download PDFInfo
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- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation process of a capacitance Frichi grid CdZnTe detector, which comprises the process steps of (1) surface treatment of CdZnTe crystals, (2) chemical corrosion, (3) electrode preparation, (4) surface passivation, (5) cleaning, (6) packaging and the like. The invention provides a preparation process for preparing a CdZnTe detector of a capacitance Frisch grid, which has simple and practical process and high resolution.
Description
Technical field
The present invention relates to the nuclear radiation detector technical field, particularly a kind of preparation technology of CdZnTe detector.
Background technology
Therefore compare with silicon (Si), germanium (Ge), tellurium zinc cadmium (CdZnTe) detector has advantages of high atomic number, high density, high resistivity and wide energy gap, can at room temperature work, detection efficient is high, leakage current is little, and noise is low.For the high-energy radiation in universe (0.5-10MeV), the CdZnTe detector has stronger radiation resistance and better adaptability, therefore compound semiconductor CdZnTe detector is more suitable for the space flight by Seeds of First Post-flight, for " space X, gamma-ray detection " this field in space physics and astrophysics research provides that energy spectrum performance is good, spatial resolution and high Satellite-borne Detector and the spectrometer of angular resolution.
the CdZnTe detector also has following shortcoming: the impurity of CdZnTe monocrystalline and defective form the trapping center in electronics and hole, in addition due to the physical characteristic of CdZnTe---the mobility in hole and life-span are than a little order of magnitude of electronics, cause the trapping in hole in charge-trapping and transmitting procedure more serious than electronics, these 2 cause the CdZnTe detector that electronics and hole are collected not exclusively, have the smearing that more serious hole trapping causes, what and the thickness of detector of also causing simultaneously induced charge on collector (anode), electron drift length, hole drift length is relevant, namely and χ, gamma-rays is absorbed the position of decay in the CdZnTe detector relevant, impact is to χ, the energy resolution that energy of γ ray is analyzed, enabling the spectrum peak amplitude reduces, the low energy side is raised and broadening.The CdZnTe detector of planar electrode structure can not meet the requirement to high energy resolution, therefore for addressing these problems, derive multiple electrode structure on the basis of CdZnTe planar electrode structure, as common flat grate electrode structure, CapturePlus electrode structure, dome-type electrode structure and electric capacity Frisch gate electrode structure.The inventor has determined the principle of the redistribution of charge inducing between electrode according to the geometry of single electric charge carrier collection principle and electrode, thereby change the weight potential field by changing electrode structure, consist of and only to collect single electric charge carrier detector of electronics and ignore the signal that the hole produces, like this electric charge of measurement just with location independent.The energy resolution that in these unipolarity electrode structures, the preparation technology of electric capacity Frisch grid detector can larger raising detector, and the simplest, also more easily realize.
At present, detector preparation method about electric capacity Frisch grid structure has many kinds, for example, the preparation method of CZT detector is briefly disclosed in " room temperature CdZnTe nuclear radiation detector progress " literary composition in " semiconductor technology " the 33rd volume o. 11th in 2008, the method (1) does not provide the matched proportion density of passivating solution, and (2) sputtering method prepares electrode can produce damage at plane of crystal." nuclear electronics and Detection Techniques " the 28th volume the 4th in 2008 is interim, and " " only disclose conventional technological process in a literary composition, detailed processing step is not reported in the preparation of CdZnTe nuclear radiation detector.
Summary of the invention
The present invention has overcome deficiency of the prior art, provides a kind of technique simple, practical, the preparation technology of the electric capacity Frisch grid CdZnTe detector that the resolution of the CdZnTe detector of preparing is high.
In order to solve the problems of the technologies described above, the present invention is achieved by the following scheme:
The preparation technology of a kind of electric capacity Frisch grid CdZnTe detector, the processing step such as surface treatment, (2) chemical corrosion, the preparation of (3) electrode, (4) surface passivation, (5) cleaning, (6) encapsulation that comprises (1) CdZnTe crystal, wherein:
(1) surface treatment: the diamond dust that adopts different model is grinding and polishing CdZnTe crystal repeatedly, and ground CdZnTe crystal is stand-by with deoil ultrasonic cleaning, deionized water ultrasonic cleaning, oven dry of acetone;
(2) chemical corrosion: the anode region of anode surface is covered layer protecting film, the CdZnTe crystal that is coated with diaphragm is placed in the chemical corrosion of bromine methanol solution, then the methyl alcohol cancellation of the sample after corrosion washes diaphragm, cleans the CdZnTe crystal;
(3) electrode preparation: zone and negative electrode at CdZnTe crystal anode covered with protective film plate Au with Vacuum Coating method, make annode area less than cathode area;
(4) surface passivation: will be placed in ammonium fluoride (NH through the CdZnTe crystal after step (3)
4F), soak in the mixed solution of deionized water and hydrogen peroxide, the ammonium fluoride (NH in mixed solution wherein
4F), the ratio of deionized water and hydrogen peroxide is 2.68g: 17ml: 8ml;
(5) clean: use deionized water ultrasonic cleaning, methanol dehydration, oven dry after passivation;
(6) encapsulation: adopt dielectric film and copper film to be centered around crystal on side face and consist of the electric capacity grid, draw detector electrodes.
The present invention is all right:
Constant temperature is aging in described step (5) is placed on baking oven.Described step (4) surface passivation 5～30 minutes.Described step (2) chemical corrosion 1～10 minute in the bromine methanol solution.In bromine methanol solution in described step (2), bromine content is 2%～5%.Use before heat, cold all apparatus of washed with de-ionized water in step (1).Adopt constant temperature, rotation CdZnTe crystal at the uniform velocity in the chemical corrosion process of described step (2).Described diaphragm is black wax.The resistance value of the deionized water in described step (4) 〉=2M Ω.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention makes the detector energy resolution of preparing better the organic combination of step of the processing of CdZnTe plane of crystal, chemical corrosion, electrode preparation, surface passivation, cleaning, encapsulation, and energy resolution is better than 3% to 662kev.After cleaning, the CdZnTe crystal is placed in baking oven constant temperature aging, makes the performance of detection more stable, longer service life.The present invention can improve detector applying bias value and reduce simultaneously the detector leakage current, strengthened on the other hand the CdZnTe detector the inside field intensity, reduce detector electric capacity.Encapsulation increases the length of Frisch's grid, can strengthen like this weight potential field of anode annex, makes the duplet detector output signal play main contributions, and effectively reducing the hole trapping affects power spectrum.
Description of drawings
Fig. 1 process chart
Fig. 2 detector schematic cross-section
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
Preparation before the technique preparation
Clean all apparatus.Use respectively heat, cold deionized water rinsing clean, the micronic dust or the ion that prevent from being attached on apparatus stain the CdZnTe material.
1.CdZnTe plane of crystal is processed
With the diamond dust of different size model grinding and polishing CdZnTe crystal repeatedly, that removes surface oxide layer and plane of crystal draws road, damage.With the acetone ultrasonic cleaning of deoiling, the deionized water ultrasonic cleaning is until the resistance value of deionized water 〉=1.5M Ω post-drying is stand-by with ground CdZnTe crystal.The present embodiment adopts respectively W10, W7, W5, W3.5 to grind successively.
2. chemical etch polishing
Originally be the chemical etch polishing liquid that embodiment adopts---bromine methanol solution: 2%～5% bromine, corroded 1～10 minute.
The annode area of the present invention's preparation is less than cathode area; the anode region of anode surface covers layer protecting film to protect this part not by chemical corrosion; the methyl alcohol cancellation of sample after corrosion; because the active height of the CdZnTe sample surfaces that takes out from etchant solution is easily oxidized; if directly be exposed in air; can generate inhomogeneous oxide layer; therefore should put into immediately methyl alcohol; use again deionized water (resistance value 〉=2M Ω) ultrasonic irrigation repeatedly instead; until then the resistance value of deionized water 〉=3M Ω gets rid of diaphragm.Diaphragm in the present embodiment adopts black wax, then dissolves black wax with trichloroethylene, with the trichloroethylene of acetone soln dissolving sample face surface attachment, uses at last the deionized water ultrasonic cleaning, protected like this part with form mesa structure on every side.
In the process of corrosion, the bromine methanol solution keeps constant temperature and uniform rotation sample, can prevent that like this etch pit or corrosion layer from appearring in the surface, affects the energy spectrum characteristics of detector.
Chemical etching technology requires very high to the cleanliness factor of the apparatus such as the corrosion clamp that uses, polytetrafluoroethylcontainer container, beaker.
The sample of wash clean takes out on superclean bench, dries up with dry argon gas, puts into immediately preprepared vacuum evaporation bell jar, vacuumizes.Purpose is to reduce as far as possible the spontaneous oxidation of sample, affects the processability of the follow-up surface electrode of detector.
Chemical etch polishing can be removed damage and the defective that stays at the CdZnTe sample surfaces on the one hand after the operations such as mechanical lapping, polishing, improve the evenness of polished surface; On the other hand, adopt the etch polishing liquid of different agent combination.Crystal face beyond chemical etch polishing, also different at electrode lower surface recombination rate, even difference is very large, thereby impact to the collection in electronics, hole, the performance that detector will obtain just must be noted that to prepare the face of electrode and the plane of incidence of nuclear radiation.Must fall skim to the wafer surface homogeneous corrosion after grinding in experiment, this is a step very crucial in the detector preparation process, because the wafer surface characteristics after corrosion directly has influence on the collection characteristic of tracking current and the electric charge of detector.
3. electrode preparation
The present embodiment adopts the method for vacuum coating, and the CdZnTe plane of crystal mask film covering after chemical etch polishing deposits afterwards Au and forms Ohm contact electrode, obtains annode area less than primary anode structure and the mesa structure of cathode area.Although the electron gun sputtering method is more advanced, the membrane electrode surface adhesion force that obtains is stronger, also can change the lattice structure of CdZnTe plane of crystal simultaneously, to a certain degree affects detector performance.
After CdZnTe sample after chemical corrosion fully cleans up, take out sample on superclean bench, dry up the surface with dry argon gas.After sample dries, put into immediately ready vacuum system, cover ready mask plate, adopt vacuum evaporation technology deposit layer of Au from the teeth outwards (adopting spiral helicine tungsten filament crucible during evaporation Au), vacuum degree is (5-10) * 10 approximately
-5Torr.Be to guarantee the quality of plated film, first in the situation that baffle plate preheating two or three minutes is arranged, shorten into and open again baffle plate when coccoid when metal begins fusing, strengthen electric current, gold evaporation is complete.To slowly heat during evaporation, prevent that the gold that melts is dropped on sample, damage sample surfaces, be about as the golden layer thickness that contacts use
After detector simultaneously plates, shut down and open the coating machine bell jar, the CdZnTe sample is turned over, lid the second cover mask plate, then the back side of evaporation detector.The electrode structure sectional view as shown in Figure 2.
4. surface passivation
The CdZnTe crystal is after processes is processed, and plane of crystal plays an important role to the quality of nuclear radiation detector performance, and different PROCESS FOR TREATMENT and atmosphere produce different surface states, i.e. surface conductance from the teeth outwards.The surface conductance of sample has been controlled maximum working voltage and the tracking current of detector, and the internal electric field of detector, thereby have influence on the transmission collection of electric charge and the formation of signal, detector to single electric charge carrier electrode structure, as pel array detector, common flat grate or Frisch's grid detector, plane of crystal seems particularly important to the impact of electric field.
Surface passivation is exactly the effect between insulation surfaces and reactive atmosphere, generates layer of oxide layer at the CdZnTe detector surface, makes the surface produce two interfaces, i.e. CdZnTe and oxide layer interface, oxide layer and atmosphere interface on every side.Therefore good surface passivation technology can improve surface stability, reduces surface conductance, reduces surface recombination, and the surface is reduced to minimum to the impact of charge transmission and collection, reaches the purpose that improves detector performance.
The surface passivation method of the present invention's employing is the approximately oxide layer of the even compact of tens nanometers of thick layer of directly growing from the teeth outwards, considers passivating dip to not damage of gold electrode, so uses ammonium fluoride (NH after preparing electrode
4F), the mixed liquid dipping sample of deionized water and hydrogen peroxide, ratio is 2.68g: 17ml: 8ml, 5～30 minutes, the deionized water of the resistance value of the preferred deionized water of the present embodiment 〉=2M Ω.Sample surfaces beyond electrode presents the passivated surface of pitch-dark light like this.
After passivation with deionized water clean up, methanol dehydration, oven dry.
6. the present embodiment before encapsulation, carries out burin-in process to the CdZnTe detector, is placed in the baking oven of 50 ℃～125 ℃ constant temperature 2～3 hours.
7. encapsulation
After the sample passivation, be centered around crystal on side face with dielectric film and copper film and consist of the electric capacity grid, the length of grid is increased to and the detector consistency of thickness, plays simultaneously the effect of package casing protection detector, draws detector electrodes.
The present embodiment preferably adopts novel Frisch grid structure, the height of Frisch's grid is extended to the whole height of CdZnTe crystal, and with separating between a thin dielectric and CdZnTe crystal, applied electric field is not corrected, and sets up a new weight potential field on detector.Not only the leakage current of detector do not had the essence impact, and strengthened near the weight potential field anode, improve charge collection efficiency, improve energy resolution.
Claims (9)
1. the preparation technology of an electric capacity Frisch grid CdZnTe detector, the processing step such as surface treatment, (2) chemical corrosion, the preparation of (3) electrode, (4) surface passivation, (5) cleaning, (6) encapsulation that comprises (1) CdZnTe crystal, it is characterized in that
(1) surface treatment: the diamond dust that adopts different model is grinding and polishing CdZnTe crystal repeatedly, and ground CdZnTe crystal is stand-by with deoil ultrasonic cleaning, deionized water ultrasonic cleaning, oven dry of acetone;
(2) chemical corrosion: the anode region of anode surface is covered layer protecting film, the CdZnTe crystal that is coated with diaphragm is placed in the chemical corrosion of bromine methanol solution, then the methyl alcohol cancellation of the sample after corrosion washes diaphragm, cleans the CdZnTe crystal;
(3) electrode preparation: zone and negative electrode at CdZnTe crystal anode covered with protective film plate Au with Vacuum Coating method, make annode area less than cathode area;
(4) surface passivation: will be placed in ammonium fluoride (NH through the CdZnTe crystal after step (3)
4F), in the mixed solution of deionized water and hydrogen peroxide, the ammonium fluoride (NH in mixed solution wherein
4F), the ratio of deionized water and hydrogen peroxide is 2.68g: 17ml: 8ml;
(5) clean: use deionized water ultrasonic cleaning, methanol dehydration, oven dry after passivation;
(6) encapsulation: adopt dielectric film and copper film to be centered around crystal on side face and consist of the electric capacity grid, draw detector electrodes.
2. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, constant temperature is aging in described step (5) is placed on baking oven.
3. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that described step (4) surface passivation 5～30 minutes.
4. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, described step (2) chemical corrosion 1～10 minute in the bromine methanol solution.
5. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, in the bromine methanol solution in described step (2), bromine content is 2%～5%.
6. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, uses before heat, cold all apparatus of washed with de-ionized water in step (1).
7. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, adopts constant temperature, rotation CdZnTe crystal at the uniform velocity in the chemical corrosion process of described step (2).
8. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that, described diaphragm is black wax.
9. the preparation technology of a kind of electric capacity according to claim 1 Frisch grid CdZnTe detector, is characterized in that the resistance value of the deionized water in described step (4) 〉=2M Ω.
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Cited By (5)
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| CN103887370A (en) * | 2014-03-12 | 2014-06-25 | 上海电力学院 | Method for passivating surface of CdZnTe crystal |
| CN108550634A (en) * | 2018-03-15 | 2018-09-18 | 上海大学 | Using the cadmium-zinc-teiluride radiation detector and preparation method thereof of zinc oxide conductive electrode |
| CN108615786A (en) * | 2018-05-30 | 2018-10-02 | 上海大学 | Radiosensitive field-effect transistor of cadmium-zinc-teiluride and preparation method thereof |
| CN111900213A (en) * | 2020-08-04 | 2020-11-06 | 上海大学 | CdMnTe imaging detector and preparation method thereof |
| CN112349797A (en) * | 2020-10-13 | 2021-02-09 | 上海大学 | Device structure of cadmium zinc telluride detector and preparation process thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887370A (en) * | 2014-03-12 | 2014-06-25 | 上海电力学院 | Method for passivating surface of CdZnTe crystal |
| CN103887370B (en) * | 2014-03-12 | 2016-03-30 | 上海电力学院 | A kind of passivating method of tellurium-zincium-cadmium crystal surface |
| CN108550634A (en) * | 2018-03-15 | 2018-09-18 | 上海大学 | Using the cadmium-zinc-teiluride radiation detector and preparation method thereof of zinc oxide conductive electrode |
| CN108615786A (en) * | 2018-05-30 | 2018-10-02 | 上海大学 | Radiosensitive field-effect transistor of cadmium-zinc-teiluride and preparation method thereof |
| CN111900213A (en) * | 2020-08-04 | 2020-11-06 | 上海大学 | CdMnTe imaging detector and preparation method thereof |
| CN111900213B (en) * | 2020-08-04 | 2022-06-14 | 上海大学 | Preparation method of CdMnTe imaging detector |
| CN112349797A (en) * | 2020-10-13 | 2021-02-09 | 上海大学 | Device structure of cadmium zinc telluride detector and preparation process thereof |
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