CN103219422A - Method for preparing CdZnTe film ultraviolet light detector with ohm structure - Google Patents
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Abstract
The invention relates to a method for preparing a CdZnTe film ultraviolet light detector with an ohm structure, which belongs to the technical field of manufacturing techniques of inorganic non-metal material devices. According to the method, a CdZnTe film is prepared by adopting a close-spaced sublimation method, and the ultraviolet light detector with a CdZnTe film ohm structure is manufactured, so that a novel method for manufacturing a high-performance ultraviolet light detector is provided. Due to the adoption of the method, a CdZnTe film sample with high flatness, uniform particle size and high resistivity is prepared. The thickness of the film is over 300 meters, and the resistance is over 109 omega centimeters.
Description
Technical field
The present invention relates to a kind of manufacture method of ohm configuration CdZnTe thin film ultraviolet detector, belong to technical for fabricating parts in inorganic non-metal.
Background technology
The ultraviolet detection technology is to study the most popular dual-use detecting technique in recent years.Because cosmic space, flame, oil, gas pollutant molecule, and the corona phenomenon of high-voltage line etc. all can contain ultraviolet radiation, so the ultraviolet detector demand that all has a wide range of applications in fields such as space flight, communication, civilian detections.Countries in the world are classified solid-state ultraviolet detector technology as the emphasis problem of current research and development.In the research of wide bandgap semiconductor ultraviolet detector, past 10 years mainly concentrated on the materials such as SiC, GaN, ZnO, diamond thin.In recent years, the progress that obtains with thermal evaporation techniques growth " detector grade " CdZnTe film aspect had caused the researchers' of field of detecting very big interest.
CdZnTe is important
-
Compound semiconductor because it has higher average atomic number and bigger energy gap, so have bigger absorption coefficient, higher counting rate with the detector of this material preparation, does not especially need any cooling device just can at room temperature work.The photoelectric properties that it is superior can be widely used in x-ray fluorescence analysis, safety detection, medical imaging and space research.But because the intrinsic rerum natura of CdZnTe, the crystal of melt method for growing exists uneven components, crystal boundary, twin, dislocation, is mingled with and precipitates and equates many defectives, and the CdZnTe monocrystal material is not suitable for the large-area flat-plate detector.For this reason, we will seek a kind of suitable large tracts of land CdZnTe film, method that cost is low of preparing.
It is simple that thin film preparation process is compared monocrystalline growing process, and cost is lower, the feasibility height of growing in batches, and the flatness of the response of based thin film is fit to the large-area flat panel detector of preparation.At present in the world the research of CdZnTe thin film detector still is in the starting stage.The CdZnTe film can be prepared by chemical method, also can obtain by physical vapour deposition (PVD).In these method for manufacturing thin film, the near space sublimed method is the most promising a kind of method, and this method cost is low, speed is fast, quality good, is applicable to large-area film deposition.At present, the near space sublimed method has been used for the preparation of CdTe film, but does not see its application on the CdZnTe thin film detector.
Adopt the near space sublimation apparatus to prepare the CdZnTe film, the grain size of film surface, density, evenness can be controlled by operating air pressure, so that improve the resistivity of CdZnTe film surface, reduce leakage current with this.The electrode structure energy better controlled leakage current of ohmic contact reduces noise, improves the linear responsiveness of device.In view of the CdZnTe thin film detector have work under spatial discrimination height, detection efficient height, good stability, the room temperature do not have the polarization effect, cheap and easily make advantage such as array image-forming device, be an of great value job for the research of detector grade CdZnTe thin film preparation process.Preparation technology for detector grade CdZnTe film does not study with beginning at present systematicness both at home and abroad as yet.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of ohm configuration CdZnTe thin film ultraviolet detector, adopt the near space sublimation method to prepare the CdZnTe film of surfacing, high some resistance rate, and make the ultraviolet light detector of CdZnTe film ohm configuration, provide new method for making ultraviolet light detector in high performance.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of CdZnTe thin film ultraviolet detector comprises following process and step:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5-20%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt to be coated with transparency conducting layer FTO(SnO
2: F, mix the tin oxide of fluorine) glass as substrate, with the ultrasonic cleaning 5～15 minutes respectively of deionized water, acetone and ethanol, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry with substrate;
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 1Pa, feeds argon gas air pressure is transferred to 100 ~ 500Pa, closes gas cylinder; Open Halogen lamp LED sublimation source and substrate are heated to 550 ~ 650 ℃ and 400 ~ 550 ℃ respectively; Behind growth 30min ~ 180min, feed argon gas again air pressure is transferred to 500 ~ 1000Pa, behind continued growth 30min ~ 60min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, closes mechanical pump, treats that sample is cooled to room temperature, takes out the dZnTe film sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares; Again sample 350 ~ 450 ° of C in the CdCl2 atmosphere were annealed 20 ~ 50 minutes; Compound concentration is 0.1 ~ 0.5% bromine methanol solution, immerses solution corrosion 10 ~ 60s with moving back the sample that overdoes, and obtains the CdZnTe film of surperficial rich tellurium;
(e) electrode of CdZnTe thin film detector is made: adopt evaporation or the thick metal electrode of sputtering method preparation 100 ~ 300nm at above-mentioned CdZnTe film upper surface; Then with sample in a vacuum 100 ~ 250 ° of C annealing formed good Ohmic contact in 10 ~ 60 minutes, finally make the ultraviolet light detector of CdZnTe film ohm configuration.
The present invention adopts the high fine and close CdZnTe film of near space sublimation method preparation, and is special in increasing operating pressure, prepares comparatively smooth film surface and higher resistivity.The thickness of film is 300 ~ 700mm,
Compare with prior art, the present invention has following remarkable advantage:
(1) near space sublimed method (CSS) is a kind of technology of practicality film growth, is applied in the CdTe film preparation.It is simple that near space sublimed method CdZnTe thin film preparation process is compared the CdZnTe monocrystalline growing process, and cost is lower, the feasibility height of growing in batches.
(2) can prepare the CdZnTe film of high resistivity and surface smoothness by the near space sublimed method, resistivity about 10
9Ω cm, surface roughness＜10nm.
(3) Zhi Bei sample is by corrosion, can obtain to a certain degree rich tellurium surface, this is beneficial to device and forms ohm configuration very much, the ohm configuration detector is than present CdZnTe metal ~ semiconductor ~ metal (MSM) structure detector energy better controlled device creepage, reduce noise, improve the linear responsiveness of device.
Description of drawings
Fig. 1 is the structural representation of ohm configuration CdZnTe thin film ultraviolet detector of the present invention.
Fig. 2 is the structure vertical view of ohm configuration CdZnTe thin film ultraviolet detector of the present invention.
Fig. 3 is the ultraviolet light I ~ V curve of ohm configuration CdZnTe thin film ultraviolet detector of the present invention.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
The preparation process and the step of present embodiment are as follows:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt the glass that is coated with transparency conducting layer FTO as substrate, substrate usefulness deionized water, acetone and ethanol are distinguished ultrasonic cleaning 15 minutes, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry;
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 3Pa, feeds argon gas air pressure is transferred to 200Pa, closes gas cylinder; Opening Halogen lamp LED is heated to 650 ℃ and 500 ℃ respectively with sublimation source and substrate and remains unchanged, behind the growth 150min, feed argon gas once more, air pressure is transferred to 700Pa, behind the growth 40min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, close mechanical pump, treat that sample is cooled to room temperature, take out sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares, smooth fully until the surface; Again sample 400 ° of C in the CdCl2 atmosphere were annealed 30 minutes; Compound concentration is 0.1% bromine methanol solution, immerses solution corrosion 40s with moving back the sample that overdoes, and obtains the CdZnTe film of surperficial rich tellurium, and its film thickness is 672um;
(e) make electrode: with the above-mentioned CdZnTe film upper surface that makes, the thick golden comb electrode of sputter 150nm in LDM150D ion beam sputtering instrument; Then with sample in a vacuum 200 ° of C annealing formed good Ohmic contact in 30 minutes, finally make the ultraviolet light detector of CdZnTe film ohm configuration.
Embodiment 2
The preparation process and the step of present embodiment are as follows:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt the glass that is coated with transparency conducting layer FTO as substrate, substrate usefulness deionized water, acetone and ethanol are distinguished ultrasonic cleaning 15 minutes, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry.
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 3Pa, feeds argon gas air pressure is transferred to 250Pa, closes gas cylinder; Opening Halogen lamp LED is heated to 650 ℃ and 500 ℃ respectively with sublimation source and substrate and remains unchanged, behind the growth 120min, feed argon gas once more, air pressure is transferred to 800Pa, behind the growth 50min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, close mechanical pump, treat that sample is cooled to room temperature, take out sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares, smooth fully until the surface; Again sample 400 ° of C in the CdCl2 atmosphere were annealed 30 minutes; Compound concentration is 0.2% bromine methanol solution, immerses solution corrosion 40s with moving back the sample that overdoes, and obtains the CdZnTe film of rich tellurium, and its film thickness is 573um;
(e) electrode of CdZnTe thin film detector is made: with the above-mentioned CdZnTe film upper surface that makes, and the thick golden comb electrode of sputter 150nm in LDM150D ion beam sputtering instrument.After with sample in a vacuum 200 ° of C annealing formed good Ohmic contact in 40 minutes, make the ultraviolet light detector of CdZnTe film ohm configuration.
Embodiment 3
The preparation process and the step of present embodiment are as follows:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt the glass that is coated with transparency conducting layer FTO as substrate, substrate usefulness deionized water, acetone and ethanol are distinguished ultrasonic cleaning 15 minutes, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry.
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 3Pa, feeds argon gas air pressure is transferred to 300Pa, closes gas cylinder; Opening Halogen lamp LED is heated to 650 ℃ and 400 ℃ respectively with sublimation source and substrate and remains unchanged, behind the growth 150min, feed argon gas once more, air pressure is transferred to 1000Pa, behind the growth 60min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, close mechanical pump, treat that sample is cooled to room temperature, take out sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares, smooth fully until the surface; Again sample 400 ° of C in the CdCl2 atmosphere were annealed 50 minutes; Compound concentration is 0.2% bromine methanol solution, immerses solution corrosion 60s with moving back the sample that overdoes, and obtains the CdZnTe film of rich tellurium, and its film thickness is 478um;
(e) electrode of CdZnTe thin film detector is made: with the above-mentioned CdZnTe film upper surface that makes, and the thick golden comb electrode of sputter 150nm in LDM150D ion beam sputtering instrument; Then with sample in a vacuum 200 ° of C annealing formed good Ohmic contact in 30 minutes, make the ultraviolet light detector of CdZnTe film ohm configuration.
Embodiment 4
The preparation process and the step of present embodiment are as follows:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt the glass that is coated with transparency conducting layer FTO as substrate, substrate usefulness deionized water, acetone and ethanol are distinguished ultrasonic cleaning 15 minutes, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry;
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 3Pa, feeds argon gas air pressure is transferred to 300Pa, closes gas cylinder; Opening Halogen lamp LED is heated to 650 ℃ and 400 ℃ respectively with sublimation source and substrate and remains unchanged, behind the growth 120min, feed argon gas once more, air pressure is transferred to 1000Pa, behind the growth 60min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, close mechanical pump, treat that sample is cooled to room temperature, take out sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares, smooth fully until the surface; Again sample 400 ° of C in the CdCl2 atmosphere were annealed 50 minutes; Compound concentration is 0.2% bromine methanol solution, immerses solution corrosion 60s with moving back the sample that overdoes, and obtains the CdZnTe film of rich tellurium, and its film thickness is 397um;
(e) CdZnTe monocrystalline sublimation source: with the above-mentioned CdZnTe film upper surface that makes, the thick golden comb electrode of sputter 150nm in LDM150D ion beam sputtering instrument; Then with sample in a vacuum 200 ° of C annealing formed good Ohmic contact in 40 minutes, make the ultraviolet light detector of CdZnTe film ohm configuration.
Use ultraviolet source that detector is carried out irradiation, utilize test macro such as Keithely 4200SCS semiconducting behavior sign that current signal etc. is measured test.As shown in Figure 3, to reach performance index as follows for the ultraviolet detector of this CdZnTe film ohm configuration: resistivity is about 3 * 10
9Ω cm, dark current density is less than 11 nA/mm under the 20V back bias voltage
2, density of photocurrent can reach 1600nA/mm under the UV-irradiation
2, survey very sensitive.
Claims (1)
1. the preparation method of an ohm configuration CdZnTe thin film ultraviolet detector is characterized in that, has following technical process and step:
(a) preparation of CdZnTe monocrystalline sublimation source: according to known prior art, high-purity Cd, Zn, Te are put into quartz ampoule, under high vacuum, adopt that mobile heating grows that quality is good, component distributing CdZnTe monocrystal relatively uniformly, wherein the molar content of zinc is 5-20%, and the crystal cut that growth is good is as sublimation source;
(b) substrate preliminary treatment: adopt the glass that is coated with transparency conducting layer FTO as substrate, substrate usefulness deionized water, acetone and ethanol are distinguished ultrasonic cleaning 5～15 minutes, the impurity on flush away surface and organic substance are put near space distillation reative cell after the oven dry;
(c) CdZnTe thin film growth process: open mechanical pump and vacuumize, the chamber internal gas pressure that will distil is closed mechanical pump after being evacuated to below the 1Pa, feeds argon gas air pressure is transferred to 100 ~ 500Pa, closes gas cylinder; Open Halogen lamp LED sublimation source and substrate are heated to 550 ~ 650 ℃ and 400 ~ 550 ℃ respectively; Behind growth 120min ~ 150min, feed argon gas again air pressure is transferred to 500 ~ 1000Pa, behind continued growth 40min ~ 60min, close Halogen lamp LED, opening mechanical pump, to be evacuated to air pressure be below the 10Pa, closes mechanical pump, treats that sample is cooled to room temperature, takes out sample;
(d) CdZnTe film polishing, corrosion and annealing: adopt 0.03um granularity aluminium oxide, the sample that manual polishing prepares; Again with sample at CdCl
2Annealed 20 ~ 50 minutes for 350 ~ 450 ℃ in the atmosphere; Compound concentration is 0.1 ~ 0.5% bromine methanol solution, immerses solution corrosion 10 ~ 60s with moving back the sample that overdoes, and obtains the CdZnTe film of surperficial rich tellurium;
(e) electrode of CdZnTe thin film detector is made: adopt evaporation or the thick metal electrode of sputtering method preparation 100 ~ 300nm at above-mentioned CdZnTe film upper surface; Then with sample in a vacuum 100 ~ 250 ° of C annealing formed good Ohmic contact in 10 ~ 60 minutes, finally make the ultraviolet light detector of CdZnTe film ohm configuration.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103343389A (en) * | 2013-07-05 | 2013-10-09 | 上海大学 | Preparation method for CdZnTe film with cylindrical structure |
| CN103474513A (en) * | 2013-09-26 | 2013-12-25 | 上海大学 | Method for manufacturing CdMnTe film ultraviolet-light detector of ohm structure |
| CN103500776A (en) * | 2013-09-26 | 2014-01-08 | 上海大学 | Preparation method of silica-based CdZnTe film ultraviolet light detector |
| CN103531662A (en) * | 2013-10-24 | 2014-01-22 | 上海大学 | Preparation method of ohm structure device having CdMnTe crystals grown with THM (traveling heater method) |
| CN107123698A (en) * | 2017-04-25 | 2017-09-01 | 西北工业大学 | CdZnTe planar detector surface treatment methods |
| CN108615786A (en) * | 2018-05-30 | 2018-10-02 | 上海大学 | Radiosensitive field-effect transistor of cadmium-zinc-teiluride and preparation method thereof |
| CN111883619A (en) * | 2020-08-04 | 2020-11-03 | 上海大学 | Electrode composition for nuclear radiation detector and preparation method of crystal |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103343389A (en) * | 2013-07-05 | 2013-10-09 | 上海大学 | Preparation method for CdZnTe film with cylindrical structure |
| CN103474513A (en) * | 2013-09-26 | 2013-12-25 | 上海大学 | Method for manufacturing CdMnTe film ultraviolet-light detector of ohm structure |
| CN103500776A (en) * | 2013-09-26 | 2014-01-08 | 上海大学 | Preparation method of silica-based CdZnTe film ultraviolet light detector |
| CN103531662A (en) * | 2013-10-24 | 2014-01-22 | 上海大学 | Preparation method of ohm structure device having CdMnTe crystals grown with THM (traveling heater method) |
| CN107123698A (en) * | 2017-04-25 | 2017-09-01 | 西北工业大学 | CdZnTe planar detector surface treatment methods |
| CN108615786A (en) * | 2018-05-30 | 2018-10-02 | 上海大学 | Radiosensitive field-effect transistor of cadmium-zinc-teiluride and preparation method thereof |
| CN111883619A (en) * | 2020-08-04 | 2020-11-03 | 上海大学 | Electrode composition for nuclear radiation detector and preparation method of crystal |
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Application publication date: 20130724 |