CN106567079A - Corrosive liquid for detecting dislocation of monocrystalline germanium slices and corrosion method - Google Patents
Corrosive liquid for detecting dislocation of monocrystalline germanium slices and corrosion method Download PDFInfo
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- CN106567079A CN106567079A CN201610849163.6A CN201610849163A CN106567079A CN 106567079 A CN106567079 A CN 106567079A CN 201610849163 A CN201610849163 A CN 201610849163A CN 106567079 A CN106567079 A CN 106567079A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/08—Germanium
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- General Physics & Mathematics (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
The invention discloses corrosive liquid for detecting dislocation of monocrystalline germanium slices. The corrosive liquid comprises hydrofluoric acid with the concentration being 30 wt%-50wt%, a potassium permanganate aqueous solution with the concentration being 2.9wt%-10wt%, and sulfuric acid with molar concentration being 3 mol/L -6 mol/L. The invention further discloses a corrosion method for detecting the dislocation of the monocrystalline germanium slices through the corrosive liquid. With the adoption of the corrosive liquid and the corrosion method, the dislocation of <100> and <111> monocrystalline germanium slices can be detected, and the monocrystalline slices are free of polishing, so that the problems that existing corrosive liquid can only display the dislocation through polishing and corroding in sequence, the reaction is out of control, and pollutant gas is generated can be solved; in addition, with the adoption of the method for detecting the dislocation of the monocrystalline germanium slices, the general monocrystalline germanium slices with different crystal orientations can be detected, and the simple application of a traditional corrosive can be avoided.
Description
Technical field
The invention belongs to germanium material processing technique field, and in particular to a kind of easy to operate, corrosive effect it is good for germanium
The corrosive liquid and caustic solution of single-chip dislocation detection.
Background technology
It is more next to the demand of germanium in terms of optics, electronic devices and components and clean energy resource currently due to the fast development of science and technology
It is more.The density of germanium single crystal Dislocations can have the impact of highly significant to the optically and electrically performance of material, and be different from
Silicon single crystal, is difficult to grow complete dislocation-free germanium single crystal in Ge mono crystal growth.Therefore, it is detection germanium to test germanium single crystal Dislocations
The indispensable operation of monocrystalline quality.
Generally, the method for the dislocation density in no matter testing germanium single crystal or silicon single crystal is the method for chemical preferential etch.Its
Sample before dislocation corrosion is usually cleavage surface or through the surface of chemical etch polishing rather than directly using cleaning
Cut surface, so step is comparatively laborious;Secondly, for the corrosion of different crystal orientations germanium single crystal dislocation density, need from different
Corrosive agent;Finally, adopt nitric acid as the acid of oxidisability selected corrosive agent, causing corrosion process produces the dioxy of severe toxicity more
Change nitrogen.
The content of the invention
Goal of the invention:Present invention aim at being directed to the deficiencies in the prior art, there is provided a kind of easy to operate, corrosive effect is good
And without the need for the dislocation corrosion liquid and caustic solution to the advance polishing of single germanium wafer.
Technical scheme:It is of the present invention it is a kind of for single germanium wafer dislocation detection corrosive liquid, including concentration be 30~
The hydrofluoric acid of 50wt%, concentration is the sulfuric acid that the potassium permanganate solution and molar concentration of 2.9~10wt% is 3~6mol/L,
Wherein the addition volume ratio of hydrofluoric acid, sulfuric acid and liquor potassic permanganate is 7~9:1~3:10.
Further, as the preferred version of the present invention, the corrosive liquid includes hydrofluoric acid of the concentration for 40wt%, concentration
For 5.66wt% potassium permanganate solution and molar concentration for 4mol/L sulfuric acid, wherein hydrofluoric acid, sulfuric acid and potassium permanganate
The addition volume ratio of solution is 8:1:10.
The present invention also provides a kind of caustic solution detected to single germanium wafer dislocation using above-mentioned corrosive liquid, including following step
Suddenly:
(1) dislocation corrosion liquid is prepared using hydrofluoric acid, sulfuric acid and potassium permanganate solution, and the dislocation corrosion liquid is preheated
20~60min, be heated up to 50~70 DEG C it is stand-by;
(2) successively three road cleanings are carried out to single germanium wafer surface using acetone, absolute ethyl alcohol and deionized water, is dispelled
The contamination on single germanium wafer surface;
(3) it is smooth after the single germanium wafer after cleaning is dried to be put in the dislocation corrosion liquid obtained in step (1), corrode
90~150min;
(4) single germanium wafer for completing dislocation corrosion is taken out rapidly, and is cleaned with cleaning agent 6~10 times and then be dried simultaneously
Dislocation density is detected under the microscope.
Further, the single germanium wafer is<100>Or<111>Crystal orientation single germanium wafer.
Further, the single germanium wafer is without chemically or mechanically polishing.
Further, next road cleaning is entered after single germanium wafer is dried up in every one cleaning in step (2).
Further, the cleaning agent in step (4) is deionized water.
Further, the thickness d >=500um of the single germanium wafer.
Beneficial effect:(1) corrosive liquid and caustic solution for being provided using the present invention can be right<100>With<111>Single germanium wafer
Dislocation detection is carried out, without the need for monocrystalline is polished, having broken away from existing corrosive liquid needs first to polish post-etching display dislocation, reaction
Problem that is uncontrollable, producing dusty gas;(2) dislocation detection is carried out to germanium single crystal using this method, can be to conventional difference
The germanium single crystal of crystal orientation detected, breaks away from the applicable unicity of traditional corrosive agent.
Description of the drawings
Fig. 1 is using the handling process schematic diagram detected to single germanium wafer dislocation in existing corrosive liquid and technique;
Fig. 2 is the handling process schematic diagram detected to single germanium wafer dislocation using corrosive liquid of the present invention and method.
Specific embodiment
Technical solution of the present invention is described in detail below by accompanying drawing, but protection scope of the present invention is not limited to
The embodiment.Reagent used in the present invention, without specified otherwise conventional commercial is.
Embodiment 1:A kind of corrosive liquid for the detection of single germanium wafer dislocation, including concentration is the hydrofluoric acid of 40wt%, it is dense
Spend the sulfuric acid of potassium permanganate solution and molar concentration for 5.66wt% for 4mol/L, wherein hydrofluoric acid, sulfuric acid and permanganic acid
The addition volume ratio of potassium solution is 8:1:10.
Adopt above-mentioned corrosive liquid to not polished thickness for 750um's<100>The single germanium wafer dislocation detection of crystal orientation
Caustic solution, comprises the steps:
(1) dislocation corrosion liquid is prepared using hydrofluoric acid, sulfuric acid and potassium permanganate solution, and the dislocation corrosion liquid is preheated
30min, be heated up to 60 DEG C it is stand-by;
(2) successively three road cleanings are carried out to single germanium wafer surface using acetone, absolute ethyl alcohol and deionized water, is dispelled
The contamination on single germanium wafer surface;Next road cleaning is entered after in every one cleaning single germanium wafer is dried up;
(3) it is smooth after the single germanium wafer after cleaning is dried to be put in the dislocation corrosion liquid obtained in step (1), corrode
120min;
(4) single germanium wafer for completing dislocation corrosion is taken out rapidly, and deionized water clean 8 times then be dried and
Dislocation density is detected under microscope.
Embodiment 2:The present embodiment content is essentially identical with embodiment 1, and its difference is that the single germanium wafer is<111
>The single germanium wafer of crystal orientation.
Embodiment 3:A kind of corrosive liquid for the detection of single germanium wafer dislocation, including concentration is the hydrofluoric acid of 30wt%, it is dense
Spend the sulfuric acid of potassium permanganate solution and molar concentration for 2.9wt% for 3mol/L, wherein hydrofluoric acid, sulfuric acid and potassium permanganate
The addition volume ratio of solution is 7:3:10.
Adopt above-mentioned corrosive liquid to not polished thickness for 500um's<111>The single germanium wafer dislocation detection of crystal orientation
Caustic solution, comprises the steps:
(1) dislocation corrosion liquid is prepared using hydrofluoric acid, sulfuric acid and potassium permanganate solution, and the dislocation corrosion liquid is preheated
60min, be heated up to 50 DEG C it is stand-by;
(2) successively three road cleanings are carried out to single germanium wafer surface using acetone, absolute ethyl alcohol and deionized water, is dispelled
The contamination on single germanium wafer surface;Next road cleaning is entered after in every one cleaning single germanium wafer is dried up;
(3) it is smooth after the single germanium wafer after cleaning is dried to be put in the dislocation corrosion liquid obtained in step (1), corrode
90min;
(4) single germanium wafer for completing dislocation corrosion is taken out rapidly, and deionized water clean 8 times then be dried and
Dislocation density is detected under microscope.
Embodiment 4:A kind of corrosive liquid for the detection of single germanium wafer dislocation, including concentration is the hydrofluoric acid of 50wt%, it is dense
Spend the sulfuric acid of potassium permanganate solution and molar concentration for 10wt% for 6mol/L, wherein hydrofluoric acid, sulfuric acid and potassium permanganate
The addition volume ratio of solution is 9:1:10.
Adopt above-mentioned corrosive liquid to not polished thickness for 600um's<100>The single germanium wafer dislocation detection of crystal orientation
Caustic solution, comprises the steps:
(1) dislocation corrosion liquid is prepared using hydrofluoric acid, sulfuric acid and potassium permanganate solution, and the dislocation corrosion liquid is preheated
60min, be heated up to 70 DEG C it is stand-by;
(2) successively three road cleanings are carried out to single germanium wafer surface using acetone, absolute ethyl alcohol and deionized water, is dispelled
The contamination on single germanium wafer surface;Next road cleaning is entered after in every one cleaning single germanium wafer is dried up;
(3) it is smooth after the single germanium wafer after cleaning is dried to be put in the dislocation corrosion liquid obtained in step (1), corrode
150min;
(4) single germanium wafer for completing dislocation corrosion is taken out rapidly, and deionized water clean 8 times then be dried and
Dislocation density is detected under microscope.
In existing handling process, Shou County needs to carry out chemically or mechanically polishing to single germanium wafer, then clears up
Decontamination, is then corroded using dislocation corrosion liquid, then detects single germanium wafer dislocation density, and, the position in existing process
Wrong corrosive liquid applicability is single, it is impossible to carry out dislocation corrosion for the single germanium wafer of different crystal orientations.
Binding isotherm of the present invention and reality, according to the principle of preferential etch, making the germanium single crystal of different crystal orientations can show
Come.By carrying out detecting the dislocation testing result for obtaining and existing side to single germanium wafer using corrosive liquid of the present invention and caustic solution
The correction data of the dislocation testing result that method is obtained is as shown in table 1:
The correction data of single germanium wafer dislocation testing result and existing method testing result in the embodiment 1~4 of table 1
From two groups of Data Comparisons, using the inspection of corrosive liquid of the present invention and caustic solution to the dislocation density of single germanium wafer
Survey result less with the result error of existing detection technique, and adopt the present invention overcomes needing in existing detection technique
The shortcoming of single corrosion after first polishing to single germanium wafer.
As described above, although the present invention has been represented and described with reference to specific preferred embodiment, it must not be explained
It is to the restriction of itself of the invention.Under the premise of the spirit and scope of the present invention defined without departing from claims, can be right
In the form and details various changes can be made for it.
Claims (8)
1. it is a kind of for single germanium wafer dislocation detection corrosive liquid, it is characterised in that:Including the hydrogen fluorine that concentration is 30~50wt%
Acid, concentration is the sulfuric acid that the potassium permanganate solution and molar concentration of 2.9~10wt% is 3~6mol/L, wherein hydrofluoric acid, sulphur
The addition volume ratio of acid and liquor potassic permanganate is 7~9:1~3:10.
2. it is according to claim 1 for single germanium wafer dislocation detection corrosive liquid, it is characterised in that:It is including concentration
The hydrofluoric acid of 40wt%, concentration is the sulfuric acid that the potassium permanganate solution and molar concentration of 5.66wt% are 4mol/L, wherein hydrogen
The addition volume ratio of fluoric acid, sulfuric acid and liquor potassic permanganate is 8:1:10.
3. the caustic solution that the corrosive liquid described in a kind of employing claim 1 is detected to single germanium wafer dislocation, it is characterised in that bag
Include following steps:
(1) dislocation corrosion liquid is prepared using hydrofluoric acid, sulfuric acid and potassium permanganate solution, and by dislocation corrosion liquid preheating 20~
60min, be heated up to 50~70 DEG C it is stand-by;
(2) successively three road cleanings are carried out to single germanium wafer surface using acetone, absolute ethyl alcohol and deionized water, dispels germanium list
The contamination of wafer surface;
(3) it is smooth after the single germanium wafer after cleaning is dried to be put in the dislocation corrosion liquid obtained in step (1), corrosion 90~
150min;
(4) single germanium wafer for completing dislocation corrosion is taken out rapidly, and is cleaned with cleaning agent 6~10 times and then be dried and aobvious
Dislocation density is detected under micro mirror.
4. caustic solution according to claim 3, it is characterised in that:The single germanium wafer is<100>Or<111>Crystal orientation germanium
Single-chip.
5. caustic solution according to claim 3, it is characterised in that:The single germanium wafer without chemically or mechanically polishing at
Reason.
6. caustic solution according to claim 3, it is characterised in that:By germanium list in every one cleaning in step (2)
Chip enters next road cleaning after drying up.
7. caustic solution according to claim 3, it is characterised in that:Cleaning agent in step (4) is deionized water.
8. caustic solution according to claim 1, it is characterised in that:Thickness d >=the 500um of the single germanium wafer.
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Cited By (4)
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CN107354513A (en) * | 2017-09-12 | 2017-11-17 | 中国电子科技集团公司第四十六研究所 | A kind of single germanium wafer etching process of efficient stable |
CN107604445A (en) * | 2017-09-12 | 2018-01-19 | 中国电子科技集团公司第四十六研究所 | A kind of caustic solution for improving single germanium wafer mechanical strength |
CN113188983A (en) * | 2021-04-22 | 2021-07-30 | 中国电子科技集团公司第四十六研究所 | Deviation<100>Crystal orientation 9oDislocation density measuring method for germanium single crystal wafer |
CN114606505A (en) * | 2022-03-24 | 2022-06-10 | 中锗科技有限公司 | Shellac degumming agent for infrared germanium single crystal slicing and degumming method |
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CN107354513A (en) * | 2017-09-12 | 2017-11-17 | 中国电子科技集团公司第四十六研究所 | A kind of single germanium wafer etching process of efficient stable |
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CN113188983A (en) * | 2021-04-22 | 2021-07-30 | 中国电子科技集团公司第四十六研究所 | Deviation<100>Crystal orientation 9oDislocation density measuring method for germanium single crystal wafer |
CN114606505A (en) * | 2022-03-24 | 2022-06-10 | 中锗科技有限公司 | Shellac degumming agent for infrared germanium single crystal slicing and degumming method |
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Application publication date: 20170419 |