CN104535578A - Method for rapidly revealing various defects of tellurium-zinc-cadmium crystal - Google Patents
Method for rapidly revealing various defects of tellurium-zinc-cadmium crystal Download PDFInfo
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- CN104535578A CN104535578A CN201410748015.6A CN201410748015A CN104535578A CN 104535578 A CN104535578 A CN 104535578A CN 201410748015 A CN201410748015 A CN 201410748015A CN 104535578 A CN104535578 A CN 104535578A
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Abstract
The invention discloses a method for rapidly revealing various defects of tellurium-zinc-cadmium crystal. The method comprises: firstly using a bromine methanol solution with the volume fraction of 3%-5% to perform chemical reduction on the B surface of a monocrystalline material (111) for 30-60 min, and removing a processing damaged layer of the material, so as to obtain a sample with a bright flat surface; and then using Everson corrosion liquid to disclose defects of the crystal, or using naked eyes or a common optical microscope to clearly observe various defects of the material. The advantages comprise that (1) the method is rapid and convenient, and is capable of finishing disclosure and observation on sample defects within one hour; (2) the method is wide in application scope, and is applicable to sheet-shaped, bulk and irregular samples and other various samples; (3) the method is relatively low in cost and does not need special equipment; and (4) the method does not introduce mechanical processing damage again because the chemical reagent is used for corrosion reduction.
Description
Technical field
The present invention relates to a kind of revealing method of semiconductor material crystal defect, specifically refer to the method for all kinds of defect of a kind of quick announcement tellurium-zincium-cadmium crystal.
Background technology
Tellurium zinc cadmium has excellent matching with mercury cadmium telluride in grating constant, is the first-selected substrate of HgCdTe infrared focal plane detector.In addition, tellurium zinc cadmium also can be used for preparation X and gamma ray detector, has a wide range of applications in fields such as Aid of Space Remote Sensing Technology, safety check technology, medical diagnosis technology and weaponrys.There is many unfavorable factors such as growth temperature is high, thermal conductivity is low, stacking fault energy is low, component fractional condensation due to Te-Zn-Cd monocrystal, in Te-Zn-Cd monocrystal material, inevitably there is a large amount of defect.Substrate defects can have a strong impact on homogeneity and the blind element rate of detector, reduces device performance and even causes component failure, how rapid screening high-quality Te-Zn-Cd monocrystal material tool be of great significance.
Tradition judges that the method for Te-Zn-Cd monocrystal quality of materials quality is grinding and polishing etch, first adopts mechanical lapping, mechanical buffing and chemically mechanical polishing to be removed by the machining damage layer of material surface, re-uses Everson corrosive liquid and discloses crystal defect.Machining damage layer is the defect (secondary defect) that Cdl-x_Znx_Te passes through other approach introducing except growth course, the cutting of such as monocrystalline and artificial inappropriate operation.There is following shortcoming in traditional grinding and polishing etch: (1) inefficiency, length consuming time.Because Cdl-x_Znx_Te belongs to soft hard brittle material, itself there is the characteristic that easy cleavage is cracked, low grinding pressure, low speed of grinding plate and the abrasive material compared with softwood matter can only be used to process, and the polishing processing cycle of 1 wafer was more than 1 day; (2) scope of application is little.Grinding and polishing is generally only applicable to the little bulk sample that sheet or thickness of sample are no more than 1 centimetre, cannot process under without special fixtures and process equipment for large bulk or erose sample; (3) in order to ensure machining precision, this type of grinding and polishing equipment and consumptive material are generally external import, technical know-how and cost is very high; (4) again machining damage may be introduced in grinding and polishing process.To sum up, the problem core disclosing all kinds of defect of tellurium-zincium-cadmium crystal is fast the machining damage layer removing Cdl-x_Znx_Te surface how fast, reduces costs, and expands the scope of application, also will suppress the possibility again introducing machining damage simultaneously.
Summary of the invention
Based on the relevant issues existed in current tellurium-zincium-cadmium crystal defect dipoles technology, the present invention proposes a kind of chemical reduction that utilizes and disclose the method for all kinds of defect of tellurium-zincium-cadmium crystal fast in conjunction with chemical corrosion.The bromine methanol solution that the present invention first uses volume fraction to be 3%-5%, carries out the chemical reduction of 30-60 minute to monocrystal material (111) B face, remove materials processing damage layer, obtains the sample that surface-brightening is smooth.Re-use Everson corrosive liquid and disclose the defect of crystal, with the naked eye or ordinary optical microscope just can all kinds of defects of clear observation material.
The object of the invention is in order to provide a kind of can fast, low cost, high applicability, disclose reliably the method for all kinds of defect of tellurium-zincium-cadmium crystal.Described method step is specific as follows:
(1) sample is selected: tellurium-zincium-cadmium crystal is got and obtained tellurium zinc cadmium sample to be measured along the processing of (111) face;
(2) sample is cleaned: use absolute ethyl alcohol and acetone to clean sample respectively, sample dries stand-by;
(3) prepare chemical reducer: by bromine: methyl alcohol volume ratio prepares bromine methanol solution between 3:97 to 5:95, now bromine volume fraction is between 3% to 5%, stirs stand-by;
(4) chemical reduction: faced up by sample (111) B and all immerse in chemical reduction liquid, thinning time controling is between 30-60 minute;
(5) clean sample: chemically take out sample in reducer, use absolute ethyl alcohol and deionized water to clean sample, dry up by nitrogen gun stand-by;
(6) Everson corrosive liquid is prepared: by lactic acid: nitric acid: hydrofluorite volume ratio 100:20:5 prepares Everson corrosive liquid, stirs stand-by;
(7) Everson corrosion: sample (111) B is faced up and immerses in corrosive liquid, corrosion 2.5min, then with deionized water, sample is cleaned, dry up by nitrogen gun;
(8) observe defect: sample under visible light naked eyes clearly can observe the defects such as polycrystalline, dislocation band, twin line, under an optical microscope, the Special Corrosion hole pattern produced because of crystal precipitation also can by clear resolution.
The present invention has following advantage:
(1) rapid and convenient, can complete announcement and the observation of sample defects in 1 hour.
(2) applied widely, can be used for sheet, bulk, all kinds sample such as irregular.
(3) cost is lower, and main consumptive material is chemical reagent, and does not need specialized equipment.
(4) use the thinning corrosion of chemical reagent, again can not introduce mechanical processing trauma.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of using method of the present invention.
Fig. 2 is the crystal precipitation special appearance etch pit that utilizes method described in this patent and traditional grinding and polishing etch the to disclose contrast photo at X100 optical microphotograph Microscopic observation: the rich cadmium sediment that method described in (a) this patent discloses, b rich tellurium sediment that method described in () this patent discloses, c rich cadmium sediment that () grinding and polishing etch discloses, the rich tellurium sediment that (d) grinding and polishing etch discloses.
Embodiment
Below by instantiation, the present invention is further elaborated, but preferred embodiment provided by the invention, only be used for illustrating the present invention, and scope of the present invention is not imposed any restrictions, the modifications and variations that any person skilled in the art person can realize easily include in the scope of the present invention and claims.
embodiment 1:
1 gets (111) face, edge processes the cadmium zinc telluride crystal wafer obtained.
2 is clean with the washes of absolute alcohol boiled by cadmium zinc telluride crystal wafer, then clean with acetone, and taking-up is dried stand-by.
The chemical reducer of 3 preparation: be the bromine of 99.5% by mass concentration: mass concentration be 99.7% methyl alcohol volume ratio be the proportions chemical reduction liquid of 3:97, the bromine methanol solution of the volume fraction 3% now obtained, stirs stand-by.
Sample (111) B faces up in whole immersion chemical reduction liquid by 4, and thinning time controling was at 60 minutes.
5 use absolute ethyl alcohol that wafer cleaning after chemical reduction is clean, re-use deionized water and are rinsed well by the absolute ethyl alcohol remaining in wafer surface, dry up after taking-up by nitrogen gun.
6 preparation Everson corrosive liquids: be the lactic acid of 87 ± 2% by mass concentration: mass concentration is the nitric acid of 70 ± 1%: mass concentration be 40% hydrofluorite volume ratio be the proportions Everson corrosive liquid of 100:20:5, stir stand-by.
Wafer (111) B faces up by 7 puts into corrosive liquid, corrosion 2.5min, with deionized water, wafer brush is clean after taking-up, dries up by nitrogen gun.
8 with the naked eye directly observe (111) B planar defect of material under visible light, observe and carry out Taking Pictures recording under optical microscope X50 or X100 times to the Special Corrosion hole pattern that material produces because of crystal precipitation.
embodiment 2:
1 gets (111) face, edge processes the cadmium zinc telluride crystal wafer obtained.
2 is clean with the washes of absolute alcohol boiled by cadmium zinc telluride crystal wafer, then clean with acetone, and taking-up is dried stand-by.
The chemical reducer of 3 preparation: be the bromine of 99.5% by mass concentration: mass concentration be 99.7% methyl alcohol volume ratio be the proportions chemical reduction liquid of 4:96, the bromine methanol solution of the volume fraction 4% now obtained, stirs stand-by.
Sample (111) B faces up in whole immersion chemical reduction liquid by 4, and thinning time controling was at 45 minutes.
5 use absolute ethyl alcohol that wafer cleaning after chemical reduction is clean, re-use deionized water and are rinsed well by the absolute ethyl alcohol remaining in wafer surface, dry up after taking-up by nitrogen gun.
6 preparation Everson corrosive liquids: be the lactic acid of 87 ± 2% by mass concentration: mass concentration is the nitric acid of 70 ± 1%: mass concentration be 40% hydrofluorite volume ratio be the proportions Everson corrosive liquid of 100:20:5, stir stand-by.
Wafer (111) B faces up by 7 puts into corrosive liquid, corrosion 2.5min, with deionized water, wafer brush is clean after taking-up, dries up by nitrogen gun.
8 with the naked eye directly observe (111) B planar defect of material under visible light, observe and carry out Taking Pictures recording under optical microscope X50 or X100 times to the Special Corrosion hole pattern that material produces because of crystal precipitation.
embodiment 3:
1 gets (111) face, edge processes the cadmium zinc telluride crystal wafer obtained.
2 is clean with the washes of absolute alcohol boiled by cadmium zinc telluride crystal wafer, then clean with acetone, and taking-up is dried stand-by.
The chemical reducer of 3 preparation: be the bromine of 99.5% by mass concentration: mass concentration be 99.7% methyl alcohol volume ratio be the proportions chemical reduction liquid of 5:95, the bromine methanol solution of the volume fraction 5% now obtained, stirs stand-by.
Sample (111) B faces up in whole immersion chemical reduction liquid by 4, and thinning time controling was at 30 minutes.
5 use absolute ethyl alcohol that wafer cleaning after chemical reduction is clean, re-use deionized water and are rinsed well by the absolute ethyl alcohol remaining in wafer surface, dry up after taking-up by nitrogen gun.
6 preparation Everson corrosive liquids: be the lactic acid of 87 ± 2% by mass concentration: mass concentration is the nitric acid of 70 ± 1%: mass concentration be 40% hydrofluorite volume ratio be the proportions Everson corrosive liquid of 100:20:5, stir stand-by.
Wafer (111) B faces up by 7 puts into corrosive liquid, corrosion 2.5min, with deionized water, wafer brush is clean after taking-up, dries up by nitrogen gun.
8 with the naked eye directly observe (111) B planar defect of material under visible light, observe and carry out Taking Pictures recording under optical microscope X50 or X100 times to the Special Corrosion hole pattern that material produces because of crystal precipitation.
Claims (1)
1. disclose a method for all kinds of defect of tellurium-zincium-cadmium crystal fast, it is characterized in that comprising the steps:
(1) sample is selected: tellurium-zincium-cadmium crystal is got and obtained tellurium zinc cadmium sample to be measured along the processing of (111) face;
(2) sample is cleaned: use absolute ethyl alcohol and acetone to clean sample respectively, sample dries stand-by;
(3) prepare chemical reducer: by bromine: methyl alcohol volume ratio prepares bromine methanol solution between 3:97 to 5:95, now bromine volume fraction is between 3% to 5%, stirs stand-by;
(4) chemical reduction: faced up by sample (111) B and all immerse in chemical reduction liquid, thinning time controling is between 30-60 minute;
(5) clean sample: chemically take out sample in reducer, use absolute ethyl alcohol and deionized water to clean sample, dry up by nitrogen gun stand-by;
(6) Everson corrosive liquid is prepared: by lactic acid: nitric acid: hydrofluorite volume ratio 100:20:5 prepares Everson corrosive liquid, stirs stand-by;
(7) Everson corrosion: sample (111) B is faced up and immerses in corrosive liquid, corrosion 2.5min, then with deionized water, sample is cleaned, dry up by nitrogen gun;
(8) observe defect: sample under visible light naked eyes clearly can observe the defects such as polycrystalline, dislocation band, twin line, under an optical microscope, the Special Corrosion hole pattern produced because of crystal precipitation also can by clear resolution.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105372266A (en) * | 2015-12-01 | 2016-03-02 | 中国科学院上海技术物理研究所 | Apparatus and method for fast imaging of cadmium zinc telluride wafer corrosion morphology |
| CN105466748A (en) * | 2015-12-31 | 2016-04-06 | 中铝西南铝冷连轧板带有限公司 | Detection method for surface stripes of PS baseboard |
| CN106153659A (en) * | 2016-06-21 | 2016-11-23 | 四川大学 | CdSiP2the corrosive agent of crystal and caustic solution |
| CN106546619A (en) * | 2016-11-24 | 2017-03-29 | 中国电子科技集团公司第十研究所 | A kind of grinding and polishing damage measure method of cadmium-zinc-teiluride base mercury cadmium telluride thin film |
| CN107192660A (en) * | 2017-05-27 | 2017-09-22 | 中国科学院上海技术物理研究所 | It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole |
| CN109270082A (en) * | 2018-08-09 | 2019-01-25 | 宁夏中晶半导体材料有限公司 | A method of monocrystalline silicon wafer line is determined using caustic solution and microcosmic detection |
| CN111323441A (en) * | 2020-02-24 | 2020-06-23 | 中国电子科技集团公司第十一研究所 | Tellurium-zinc-cadmium wafer screening method |
| CN112458543A (en) * | 2020-11-16 | 2021-03-09 | 西北工业大学 | Surface treatment method of CZT radiation detection thin film material |
| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
| CN115197705A (en) * | 2022-05-30 | 2022-10-18 | 北京智创芯源科技有限公司 | Etching solution and thinning method of tellurium-cadmium-mercury infrared focal plane hybrid chip |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105372266A (en) * | 2015-12-01 | 2016-03-02 | 中国科学院上海技术物理研究所 | Apparatus and method for fast imaging of cadmium zinc telluride wafer corrosion morphology |
| CN105466748A (en) * | 2015-12-31 | 2016-04-06 | 中铝西南铝冷连轧板带有限公司 | Detection method for surface stripes of PS baseboard |
| CN105466748B (en) * | 2015-12-31 | 2018-12-25 | 中铝西南铝冷连轧板带有限公司 | PS plate primary surface jail-bar detection approach |
| CN106153659A (en) * | 2016-06-21 | 2016-11-23 | 四川大学 | CdSiP2the corrosive agent of crystal and caustic solution |
| CN106153659B (en) * | 2016-06-21 | 2019-01-25 | 四川大学 | CdSiP2The corrosive agent and caustic solution of crystal |
| CN106546619A (en) * | 2016-11-24 | 2017-03-29 | 中国电子科技集团公司第十研究所 | A kind of grinding and polishing damage measure method of cadmium-zinc-teiluride base mercury cadmium telluride thin film |
| CN107192660A (en) * | 2017-05-27 | 2017-09-22 | 中国科学院上海技术物理研究所 | It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole |
| CN107192660B (en) * | 2017-05-27 | 2023-09-12 | 中国科学院上海技术物理研究所 | Device and method for dynamically observing tellurium-zinc-cadmium material chemical corrosion pits |
| CN109270082A (en) * | 2018-08-09 | 2019-01-25 | 宁夏中晶半导体材料有限公司 | A method of monocrystalline silicon wafer line is determined using caustic solution and microcosmic detection |
| CN109270082B (en) * | 2018-08-09 | 2021-05-11 | 宁夏中晶半导体材料有限公司 | Method for determining monocrystalline silicon crystal line by using corrosion method and microscopic detection |
| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
| CN111323441A (en) * | 2020-02-24 | 2020-06-23 | 中国电子科技集团公司第十一研究所 | Tellurium-zinc-cadmium wafer screening method |
| CN112458543B (en) * | 2020-11-16 | 2023-05-19 | 西北工业大学 | Surface treatment method of CZT radiation detection film material |
| CN112458543A (en) * | 2020-11-16 | 2021-03-09 | 西北工业大学 | Surface treatment method of CZT radiation detection thin film material |
| CN115197705A (en) * | 2022-05-30 | 2022-10-18 | 北京智创芯源科技有限公司 | Etching solution and thinning method of tellurium-cadmium-mercury infrared focal plane hybrid chip |
| CN115197705B (en) * | 2022-05-30 | 2023-08-15 | 北京智创芯源科技有限公司 | Etching solution and thinning method of tellurium-cadmium-mercury infrared focal plane hybrid chip |
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