CN112458543B - Surface treatment method of CZT radiation detection film material - Google Patents
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- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
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Abstract
The invention relates to a surface treatment method of a CZT radiation detection film material, which comprises the steps of preparing special rough polishing liquid and fine polishing liquid, adopting an outer 8-shaped polishing method to polish the surface of the film material, preparing special corrosive liquid, taking out after 30s of corrosion, ultrasonically cleaning for 30s by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen to finish corrosion; and then etching with oxygen ions and argon gas to finish the surface of the film material. The method improves the surface quality of the CZT polycrystalline film by polishing, corroding and etching the surface of the CZT polycrystalline thick film, and greatly improves the photoelectric performance of the thick film detector.
Description
Technical Field
The invention belongs to a surface treatment method of a film material, and particularly relates to a surface treatment method of a tellurium-zinc-cadmium semiconductor polycrystalline film material.
Background
Cd 1-x Zn x Te is a novel room temperature semiconductor nuclear radiation detector material with excellent performance, and the material has the following advantages: (1) The atomic number is large, the atomic number has relatively large blocking capacity to X-rays, a 1 mm-thick CZT wafer can fully absorb hard X-rays with energy lower than 60keV, and a 2 mm-thick CZT wafer can absorb 70% of gamma rays with energy of 122 keV; (2) Excellent carrier transport characteristics, carrier mobility and lifetime product (mu tau value) higher than 2 x 10 -3 cm 2 V; (3) The energy of the band gap is relatively wide, and the energy gap width of the room temperature is continuously adjustable between 1.49eV and 2.26 eV. Compared with a CZT wafer, the preparation of the CZT polycrystalline film can greatly reduce the cost for preparing the radiation detection device, and can prepare a flat panel detector which is uniform, compact, low in leakage current, large in switch ratio and large in area. The roughness of the film surface will affect the device performance, and typical methods for reducing the roughness of the film are: (1) The growth technological parameters are optimized in the early stage, so that the surface of the grown film is as smooth as possible, and the roughness is small; (2) But the surface of the common growing polycrystalline film is rough or has some contamination, and the surface roughness is reduced by a plurality of surface treatment methods in the later period, so that the surface leakage current is reduced, and the signal to noise ratio of the device is improved. The surface treatment is carried out on the CZT film after the growth, so that the photoelectric performance of the device can be greatly optimized.
Although the use of the CZT polycrystalline film can greatly reduce the cost of manufacturing the radiation detection device, and can manufacture flat panel detectors with uniformity, compactness, lower leakage current, larger switch and large area. However, the surface roughness of the thin film can seriously affect the performance of a device, and the surface of a CZT thick film prepared by a close-range sublimation method is uneven, the roughness is large, and the photoelectric performance of a detector prepared without surface treatment is poor.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a surface treatment method of a CZT radiation detection thin film material, which is used for polishing, corroding and etching the surface of a CZT polycrystalline thick film, so that the photoelectric performance of the thick film detector is greatly improved.
Technical proposal
A surface treatment method of a CZT radiation detection film material is characterized by comprising the following steps:
step 1, grinding: polishing the surface of the film, then ultrasonically cleaning the film by using acetone, alcohol and distilled water, and finally drying the film by using nitrogen;
step 2, rough polishing: performing rough polishing on the surface of the film by using a rough polishing liquid and adopting an external 8-shaped polishing method, and repeatedly performing ultrasonic cleaning by using distilled water until the surface has no residual white MgO; the coarse polishing solution comprises the following components: preparing coarse polishing liquid according to the mass percentage MgO:deionized=20:100;
step 3, fine polishing: performing fine polishing on the surface of the film by using a fine polishing liquid and adopting an outer 8-shaped polishing method, and performing ultrasonic cleaning for 5min by using distilled water every 20s of polishing to prevent the surface of the film from being corroded; repeating the above operation for several times; the fine polishing liquid comprises the following components: preparing a fine polishing solution according to the volume percentage of hydrogen peroxide to coarse polishing solution=1:1
Step 4, corrosion: immersing the film into corrosive liquid to corrode for 30s, taking out, then ultrasonically cleaning for 30s by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen; the corrosive liquid comprises: preparing bromomethanol corrosive liquid according to the volume percentage of methanol to bromine=50 to 1.5;
step 5, oxygen ion etching: etching the surface of the film by using a plasma etching machine, wherein the gas is oxygen, the etching power is 10W, the gas flow is 80sccm, the working air pressure is 5Pa, and the etching time is 2min;
step 6, argon etching: and etching the surface of the film by using a plasma etching machine, wherein the gas is argon, the etching power is 5W, the oxygen flow is 90sccm, the working pressure is 5Pa, and the etching time is 5min.
The surface of the polishing film in the step 1 is: the sand paper is adopted for external 8-shaped grinding and polishing.
The sand paper adopts 2000 and 5000 mesh sand paper.
The said washing with acetone, alcohol and distilled water for 20min.
The MgO powder adopts analytically pure MgO powder with purity more than that.
Advantageous effects
The surface treatment method of the CZT radiation detection film material is characterized in that special rough polishing liquid and special fine polishing liquid are prepared, the outer 8-shaped polishing method is adopted for polishing the surface of the film material, special corrosive liquid is prepared, the film material is taken out after being corroded for 30 seconds, methanol is used for ultrasonic cleaning for 30 seconds, acetone, alcohol and distilled water are used for ultrasonic cleaning for 20 minutes, and finally nitrogen is used for drying to finish corrosion; and then etching with oxygen ions and argon gas to finish the surface of the film material. The method improves the surface quality of the CZT polycrystalline film by polishing, corroding and etching the surface of the CZT polycrystalline thick film, and greatly improves the photoelectric performance of the thick film detector.
Drawings
Fig. 1: flow schematic block diagram of the present invention
Detailed Description
The invention will now be further described with reference to examples, figures:
example 1
S1, grinding: sequentially using 2000 and 5000 mesh sand paper, polishing the surface of the film by adopting an external 8-shaped polishing method until the surface of the film is flat and no obvious crystal grains can be seen by naked eyes, then ultrasonically cleaning the film for 20min by using acetone, alcohol and distilled water, and finally drying the film by using nitrogen;
s2, preparing coarse polishing liquid: mgO powder with analytical purity and above is used, and MgO is used as follows by mass percent: preparing coarse polishing solution in a ratio of deionized water=20:100;
s3, rough polishing: performing rough polishing on the surface of the film by using the rough polishing liquid prepared in the step S2 and adopting an external 8-shaped polishing method until scratches on the surface of the film cannot be observed by naked eyes, and finally repeatedly performing ultrasonic cleaning by using distilled water until no residual white MgO exists on the surface;
s4, preparing fine polishing liquid: preparing a fine polishing solution according to the volume percentage of hydrogen peroxide to the polishing solution prepared by S2=1:1;
s5, fine polishing: and (3) carrying out fine polishing on the surface of the film by using the rough polishing liquid prepared in the step (S4) and adopting an outer 8-shaped polishing method, and carrying out ultrasonic cleaning for 5min by using distilled water every 20S of polishing to prevent the surface of the film from being corroded. Repeating the above operation for several times until the lower surface is as smooth as a mirror under visual observation;
s6, preparing corrosive liquid: methanol according to volume percentage: bromine=50:1.5, preparing bromomethanol corrosive liquid;
s7, corrosion: immersing the film in the corrosive liquid prepared in the step S6, corroding for 30S, taking out, ultrasonically cleaning for 30S by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen;
s8, oxygen ion etching: etching the surface of the film by using a plasma etching machine, wherein the gas is oxygen, the etching power is 10W, the gas flow is 80sccm, the working air pressure is 5Pa, and the etching time is 2min;
s9, argon etching: and etching the surface of the film by using a plasma etching machine, wherein the gas is argon, the etching power is 5W, the oxygen flow is 90sccm, the working pressure is 5Pa, and the etching time is 5min.
Example 2
S1, grinding: sequentially using 2000 and 5000 mesh sand paper, polishing the surface of the film by adopting an external 8-shaped polishing method until the surface of the film is flat and no obvious crystal grains can be seen by naked eyes, then ultrasonically cleaning the film for 20min by using acetone, alcohol and distilled water, and finally drying the film by using nitrogen;
s2, preparing coarse polishing liquid: mgO powder with analytical purity and above is used, and MgO is used as follows by mass percent: preparing coarse polishing solution in a ratio of deionized water=20:100;
s3, rough polishing: performing rough polishing on the surface of the film by using the rough polishing liquid prepared in the step S2 and adopting an external 8-shaped polishing method until scratches on the surface of the film cannot be observed by naked eyes, and finally repeatedly performing ultrasonic cleaning by using distilled water until no residual white MgO exists on the surface;
s4, preparing fine polishing liquid: preparing a fine polishing solution according to the volume percentage of hydrogen peroxide to the polishing solution prepared by S2=1:1;
s5, fine polishing: and (3) carrying out fine polishing on the surface of the film by using the rough polishing liquid prepared in the step (S4) and adopting an outer 8-shaped polishing method, and carrying out ultrasonic cleaning for 5min by using distilled water every 20S of polishing to prevent the surface of the film from being corroded. Repeating the above operation for several times until the lower surface is as smooth as a mirror under visual observation;
s6, preparing corrosive liquid: methanol according to volume percentage: bromine=50:2, preparing bromomethanol corrosive liquid;
s7, corrosion: immersing the film in the corrosive liquid prepared in the step S6, corroding for 30S, taking out, ultrasonically cleaning for 30S by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen;
s8, oxygen ion etching: etching the surface of the film by using a plasma etching machine, wherein the gas is oxygen, the etching power is 10W, the gas flow is 80sccm, the working air pressure is 5Pa, and the etching time is 2min;
s9, argon etching: and etching the surface of the film by using a plasma etching machine, wherein the gas is argon, the etching power is 5W, the oxygen flow is 90sccm, the working pressure is 5Pa, and the etching time is 5min.
Example 3
S1, grinding: sequentially using 2000 and 5000 mesh sand paper, polishing the surface of the film by adopting an external 8-shaped polishing method until the surface of the film is flat and no obvious crystal grains can be seen by naked eyes, then ultrasonically cleaning the film for 20min by using acetone, alcohol and distilled water, and finally drying the film by using nitrogen;
s2, preparing coarse polishing liquid: mgO powder with analytical purity and above is used, and MgO is used as follows by mass percent: preparing coarse polishing solution in a ratio of deionized water=20:100;
s3, rough polishing: performing rough polishing on the surface of the film by using the rough polishing liquid prepared in the step S2 and adopting an external 8-shaped polishing method until scratches on the surface of the film cannot be observed by naked eyes, and finally repeatedly performing ultrasonic cleaning by using distilled water until no residual white MgO exists on the surface;
s4, preparing fine polishing liquid: preparing a fine polishing solution according to the volume percentage of hydrogen peroxide to the polishing solution prepared by S2=1:1;
s5, fine polishing: and (3) carrying out fine polishing on the surface of the film by using the rough polishing liquid prepared in the step (S4) and adopting an outer 8-shaped polishing method, and carrying out ultrasonic cleaning for 5min by using distilled water every 20S of polishing to prevent the surface of the film from being corroded. Repeating the above operation for several times until the lower surface is as smooth as a mirror under visual observation;
s6, preparing corrosive liquid: methanol according to volume percentage: bromine=50:1.5, preparing bromomethanol corrosive liquid;
s7, corrosion: immersing the film in the corrosive liquid prepared in the step S6, corroding for 30S, taking out, ultrasonically cleaning for 30S by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen;
s8, oxygen ion etching: etching the surface of the film by using a plasma etching machine, wherein the gas is oxygen, the etching power is 15W, the gas flow is 80sccm, the working air pressure is 5Pa, and the etching time is 10min;
s9, argon etching: and etching the surface of the film by using a plasma etching machine, wherein the gas is argon, the etching power is 10W, the oxygen flow is 90sccm, the working pressure is 5Pa, and the etching time is 10min.
Claims (5)
1. A surface treatment method of a CZT radiation detection film material is characterized by comprising the following steps:
step 1, grinding: polishing the surface of the film, then ultrasonically cleaning the film by using acetone, alcohol and distilled water, and finally drying the film by using nitrogen;
step 2, rough polishing: performing rough polishing on the surface of the film by using a rough polishing liquid and adopting an external 8-shaped polishing method, and repeatedly performing ultrasonic cleaning by using distilled water until the surface has no residual white MgO; the coarse polishing solution comprises the following components: preparing coarse polishing liquid according to the mass percentage of MgO, deionized water=20:100;
step 3, fine polishing: performing fine polishing on the surface of the film by using a fine polishing liquid and adopting an outer 8-shaped polishing method, and performing ultrasonic cleaning for 5min by using distilled water every 20s of polishing to prevent the surface of the film from being corroded; repeating the above operation for several times; the fine polishing liquid comprises the following components: preparing a fine polishing solution according to the volume percentage of hydrogen peroxide to coarse polishing solution=1:1;
step 4, corrosion: immersing the film into corrosive liquid to corrode for 30s, taking out, then ultrasonically cleaning for 30s by using methanol, ultrasonically cleaning for 20min by using acetone, alcohol and distilled water, and finally drying by using nitrogen; the corrosive liquid comprises: preparing bromomethanol corrosive liquid according to the volume percentage of methanol to bromine=50 to 1.5;
step 5, oxygen ion etching: etching the surface of the film by using a plasma etching machine, wherein the gas is oxygen, the etching power is 10W, the gas flow is 80sccm, the working air pressure is 5Pa, and the etching time is 2min;
step 6, argon etching: and etching the surface of the film by using a plasma etching machine, wherein the gas is argon, the etching power is 5W, the oxygen flow is 90sccm, the working pressure is 5Pa, and the etching time is 5min.
2. The method for surface treatment of CZT radiation detecting thin film material according to claim 1, wherein: the surface of the polishing film in the step 1 is: the sand paper is adopted for external 8-shaped grinding and polishing.
3. The surface treatment method of CZT radiation detecting thin film material according to claim 2, wherein: the sand paper adopts 2000 and 5000 mesh sand paper.
4. The method for surface treatment of CZT radiation detecting thin film material according to claim 1, wherein: in the first step, acetone, alcohol and distilled water are used for ultrasonic cleaning for 20min.
5. The method for surface treatment of CZT radiation detecting thin film material according to claim 1, wherein: the MgO powder adopts analytically pure MgO powder with purity more than that.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104535578A (en) * | 2014-12-09 | 2015-04-22 | 中国科学院上海技术物理研究所 | Method for rapidly revealing various defects of tellurium-zinc-cadmium crystal |
| CN107123698A (en) * | 2017-04-25 | 2017-09-01 | 西北工业大学 | CdZnTe planar detector surface treatment methods |
| CN110289215A (en) * | 2019-06-25 | 2019-09-27 | 上海大学 | The inductively coupled plasma etching process of tellurium-zincium-cadmium crystal |
| CN110299287A (en) * | 2019-06-24 | 2019-10-01 | 上海大学 | The processing of surface polishing method of tellurium zincium vestalium thin-film |
| CN111834229A (en) * | 2020-07-23 | 2020-10-27 | 大连理工大学 | Environment-friendly chemical mechanical polishing method for cadmium zinc telluride wafer |
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| GB2474720A (en) * | 2009-10-26 | 2011-04-27 | Finphys Oy | Neutron Detector |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535578A (en) * | 2014-12-09 | 2015-04-22 | 中国科学院上海技术物理研究所 | Method for rapidly revealing various defects of tellurium-zinc-cadmium crystal |
| CN107123698A (en) * | 2017-04-25 | 2017-09-01 | 西北工业大学 | CdZnTe planar detector surface treatment methods |
| CN110299287A (en) * | 2019-06-24 | 2019-10-01 | 上海大学 | The processing of surface polishing method of tellurium zincium vestalium thin-film |
| CN110289215A (en) * | 2019-06-25 | 2019-09-27 | 上海大学 | The inductively coupled plasma etching process of tellurium-zincium-cadmium crystal |
| CN111834229A (en) * | 2020-07-23 | 2020-10-27 | 大连理工大学 | Environment-friendly chemical mechanical polishing method for cadmium zinc telluride wafer |
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