CN105483833A - Dislocation etching method for aluminum nitride single crystal - Google Patents
Dislocation etching method for aluminum nitride single crystal Download PDFInfo
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- CN105483833A CN105483833A CN201510820250.4A CN201510820250A CN105483833A CN 105483833 A CN105483833 A CN 105483833A CN 201510820250 A CN201510820250 A CN 201510820250A CN 105483833 A CN105483833 A CN 105483833A
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- single crystal
- nitride single
- aluminum
- dislocation
- deionized water
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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
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
Abstract
The invention discloses a dislocation etching method for an aluminum nitride single crystal. The dislocation etching method comprises the following steps: 1) subjecting an aluminum nitride single crystal wafer to ultrasonic cleaning with an organic solvent; 2) subjecting the aluminum nitride single crystal wafer to immersion cleaning with an organic solvent; 3) flushing the surface of the aluminum nitride single crystal wafer with deionized water; 4) putting the aluminum nitride single crystal wafer in a chemical etching solution and carrying out dislocation etching at 300 to 400 DEG C; 5) flushing the aluminum nitride single crystal wafer etched in the step 4) with deionized water; and 6) drying the aluminum nitride single crystal wafer. The dislocation etching method provided by the invention has high etching efficiency and good process controllability and can rapidly and clearly display dislocation.
Description
Technical field
The present invention relates to field of semiconductor materials, particularly relate to a kind of dislocation corrosion method of Group III-V compound semiconductor material aluminium nitride.
Background technology
Aluminium nitride material is the later third generation novel semiconductor material of the materials such as first-generation silicon, germanium and s-generation gallium arsenide, indium phosphide that continues.Aluminum-nitride single crystal material has the advantages such as broad stopband, high heat conductance, high temperature resistant, high breakdown field strength, it is the base mateiral of preparation high-performance deep ultraviolet detector, HIGH-POWERED MICROWAVES device and electron device, novel microwave device, for meeting device miniaturization, high temperature resistant, powerful requirement, must use aluminum-nitride single crystal material to make AlGaN homepitaxy fine structure material.The dislocation desity of monocrystal material has decisive influence for the quality of its performance and epitaxial material, is therefore necessary to carry out furtheing investigate to obtain high-quality aluminum-nitride single crystal material for material Dislocations.
Summary of the invention
For Problems existing in background technology, the object of the present invention is to provide a kind of dislocation corrosion method of aluminum-nitride single crystal, this dislocation corrosion method corrosion efficiency is high, technology controlling and process performance is good; And dislocation can be shown fast, clearly.
The object of the invention is to be achieved through the following technical solutions:
A dislocation corrosion method for aluminum-nitride single crystal, described dislocation corrosion method comprises the steps:
1) organic solvent ultrasonic cleaning is carried out to aluminum-nitride single crystal sheet;
2) carry out organic solvent to described aluminum-nitride single crystal sheet to embathe;
3) with the surface of aluminum-nitride single crystal sheet described in deionized water rinsing;
4) described aluminum-nitride single crystal sheet is put into chemical corrosion liquid, under the temperature condition of 300-400 DEG C, carry out dislocation corrosion;
5) with the aluminum-nitride single crystal sheet after corrosion in deionized water rinsing step 4);
6) dry described aluminum-nitride single crystal sheet.
Further, the described organic solvent in step 1) is acetone, and the time of described ultrasonic cleaning is 10-20 minute, cleaning temperature 30-40 DEG C.
Further, step 2) in described organic solvent be alcohol, the time of embathing is 20-30 minute, and temperature is 30-40 DEG C.
Further, the deionized water rinsing method in step 3) is specially: to rinse described aluminum-nitride single crystal sheet surperficial with arrange the mode that combines of washing by water soon to use deionized water overflow rinsing, and flush time is 30 seconds to 2 minutes, and in addition manual flush operates again afterwards.
Further in molten state sodium hydroxide, the potassium hydroxide of, the chemical corrosion liquid in step 4) to be mass percent be 1:1, use silver crucible, etching time is 3-20 minute, corrosion temperature 300-400 DEG C.
Further, the deionized water rinsing method in step 5) is specially: to rinse described aluminum-nitride single crystal sheet surperficial with arrange the mode that combines of washing by water soon to use deionized water overflow rinsing, and flush time is 30 seconds to 2 minutes, and in addition manual flush operates again afterwards.
Further, in step 6), drying process is: by described aluminum-nitride single crystal sheet dry 30-90 second at the temperature of 50-60 DEG C.
The present invention has following positive technique effect:
The dislocation corrosion method corrosion efficiency of the application is high, technology controlling and process performance is good; And dislocation can be shown fast, clearly.
Accompanying drawing explanation
Aluminum nitride crystal (0001) face that Fig. 1 is through method of the present invention corrosion demonstrates obvious sexangle dislocation schematic diagram under an optical microscope.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Be that the square aluminum-nitride single crystal sheet of 10mm × 10mm of 1mm puts into hand basket by a slice thickness, hand basket immersed and fills in the ultrasonic cleaning tank of acetone soln, under 30 DEG C of conditions, ultrasonic cleaning 10 minutes.Afterwards hand basket is immersed in spirituous solution, under 30 DEG C of conditions, embathe 20 minutes.Immediately hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with soon arrange the mode combined of washing by water and rinse 30 seconds, and in addition manual flush 10 seconds.Afterwards hand basket is immersed in molten sodium hydroxide that 1:1 in mass ratio prepares, potassium hydroxide mixed solution, corrode 5 minutes under 300 DEG C of conditions, again hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with arranging the mode combined of washing by water rinses 60 seconds soon, and in addition manual flush 10 seconds, afterwards aluminium nitride wafer is put into wafer rotary drier, dry with hot nitrogen, drying temperature 50 DEG C, 30 seconds time of drying.
Embodiment 2
Be that the square aluminum-nitride single crystal sheet of 10mm × 10mm of 1mm puts into hand basket by a slice thickness, hand basket immersed and fills in the ultrasonic cleaning tank of acetone soln, under 35 DEG C of conditions, ultrasonic cleaning 15 minutes.Afterwards hand basket is immersed in spirituous solution, under 35 DEG C of conditions, embathe 25 minutes.Immediately hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with soon arrange the mode combined of washing by water and rinse 60 seconds, and in addition manual flush 10 seconds.Afterwards hand basket is immersed in molten sodium hydroxide that 1:1 in mass ratio prepares, potassium hydroxide mixed solution, corrode 15 minutes under 350 DEG C of conditions, again hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with arranging the mode combined of washing by water rinses 90 seconds soon, and in addition manual flush 10 seconds, afterwards aluminium nitride wafer is put into wafer rotary drier, dry with hot nitrogen, drying temperature 55 DEG C, 60 seconds time of drying.
Embodiment 3
Be that the square aluminum-nitride single crystal sheet of 10mm × 10mm of 1mm puts into hand basket by a slice thickness, hand basket immersed and fills in the ultrasonic cleaning tank of acetone soln, under 40 DEG C of conditions, ultrasonic cleaning 20 minutes.Afterwards hand basket is immersed in spirituous solution, under 40 DEG C of conditions, embathe 30 minutes.Immediately hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with soon arrange the mode combined of washing by water and rinse 90 seconds, and in addition manual flush 10 seconds.Afterwards hand basket is immersed in molten sodium hydroxide that 1:1 in mass ratio prepares, potassium hydroxide mixed solution, corrode 20 minutes under 400 DEG C of conditions, again hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with arranging the mode combined of washing by water rinses 110 seconds soon, and in addition manual flush 10 seconds, afterwards aluminium nitride wafer is put into wafer rotary drier, dry with hot nitrogen, drying temperature 60 DEG C, 90 seconds time of drying.
Preferred embodiment
Be that the square aluminum-nitride single crystal sheet of 10mm × 10mm of 1mm puts into hand basket by a slice thickness, hand basket immersed and fills in the ultrasonic cleaning tank of acetone soln, under 30 DEG C of conditions, ultrasonic cleaning 15 minutes.Afterwards hand basket is immersed in spirituous solution, under 35 DEG C of conditions, embathe 15 minutes.Immediately hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with soon arrange the mode combined of washing by water and rinse 30 seconds, and in addition manual flush 10 seconds.Afterwards hand basket is immersed in molten sodium hydroxide that 1:1 in mass ratio prepares, potassium hydroxide mixed solution, corrode 5 minutes under 300 DEG C of conditions, again hand basket is inserted afterwards in over flow rinse groove, with deionized water overflow rinsing with arranging the mode combined of washing by water rinses 60 seconds soon, and in addition manual flush 10 seconds, afterwards aluminium nitride wafer is put into wafer rotary drier, dry with hot nitrogen, drying temperature 60 DEG C, 30 seconds time of drying.
Aluminum-nitride single crystal of the present invention (0001) face dislocation photo adopts Olympus Optical microscope photographing.
Described just in order to the present invention is described above, be construed as the present invention and be not limited to above embodiment, meet the various variants of inventive concept all within protection scope of the present invention.
Claims (7)
1. a dislocation corrosion method for aluminum-nitride single crystal, is characterized in that, described dislocation corrosion method comprises the steps:
1) organic solvent ultrasonic cleaning is carried out to aluminum-nitride single crystal sheet;
2) carry out organic solvent to described aluminum-nitride single crystal sheet to embathe;
3) with the surface of aluminum-nitride single crystal sheet described in deionized water rinsing;
4) described aluminum-nitride single crystal sheet is put into chemical corrosion liquid, under the temperature condition of 300-400 DEG C, carry out dislocation corrosion;
5) with the aluminum-nitride single crystal sheet after corrosion in deionized water rinsing step 4);
6) dry described aluminum-nitride single crystal sheet.
2. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, is characterized in that, the described organic solvent in step 1) is acetone, and the time of described ultrasonic cleaning is 10-20 minute, cleaning temperature 30-40 DEG C.
3. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, is characterized in that, step 2) in described organic solvent be alcohol, the time of embathing is 20-30 minute, and temperature is 30-40 DEG C.
4. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, it is characterized in that, deionized water rinsing method in step 3) is specially: use deionized water overflow rinsing to rinse described aluminum-nitride single crystal sheet surface with the fast mode combined of washing by water of arranging, flush time is 30 seconds to 2 minutes, afterwards in addition manual flush operation again.
5. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, it is characterized in that, molten state sodium hydroxide, the potassium hydroxide of to be mass percent the be 1:1 of the chemical corrosion liquid in step 4), use silver crucible, etching time is 3-20 minute, corrosion temperature 300-400 DEG C.
6. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, it is characterized in that, deionized water rinsing method in step 5) is specially: use deionized water overflow rinsing to rinse described aluminum-nitride single crystal sheet surface with the fast mode combined of washing by water of arranging, flush time is 30 seconds to 2 minutes, afterwards in addition manual flush operation again.
7. the dislocation corrosion method of aluminum-nitride single crystal according to claim 1, is characterized in that, in step 6), drying process is: by described aluminum-nitride single crystal sheet dry 30-90 second at the temperature of 50-60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510820250.4A CN105483833A (en) | 2015-11-24 | 2015-11-24 | Dislocation etching method for aluminum nitride single crystal |
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| CN201510820250.4A CN105483833A (en) | 2015-11-24 | 2015-11-24 | Dislocation etching method for aluminum nitride single crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106480508A (en) * | 2016-12-22 | 2017-03-08 | 苏州奥趋光电技术有限公司 | A kind of wet etch processor for aluminum nitride crystal |
| CN107829144A (en) * | 2017-10-20 | 2018-03-23 | 苏州奥趋光电技术有限公司 | A kind of wet corrosion technique for aluminum nitride crystal |
| CN108381379A (en) * | 2018-04-13 | 2018-08-10 | 中国电子科技集团公司第四十六研究所 | The polishing method that aluminum-nitride single crystal piece electrobrightening and chemically mechanical polishing are combined |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106480508A (en) * | 2016-12-22 | 2017-03-08 | 苏州奥趋光电技术有限公司 | A kind of wet etch processor for aluminum nitride crystal |
| CN107829144A (en) * | 2017-10-20 | 2018-03-23 | 苏州奥趋光电技术有限公司 | A kind of wet corrosion technique for aluminum nitride crystal |
| CN108381379A (en) * | 2018-04-13 | 2018-08-10 | 中国电子科技集团公司第四十六研究所 | The polishing method that aluminum-nitride single crystal piece electrobrightening and chemically mechanical polishing are combined |
| CN108381379B (en) * | 2018-04-13 | 2019-05-24 | 中国电子科技集团公司第四十六研究所 | The polishing method that aluminum-nitride single crystal piece electrobrightening and chemically mechanical polishing combine |
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