CN110205681B - Dislocation corrosion liquid for indium arsenide single crystal wafer and dislocation corrosion detection method - Google Patents

Dislocation corrosion liquid for indium arsenide single crystal wafer and dislocation corrosion detection method Download PDF

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CN110205681B
CN110205681B CN201910479476.0A CN201910479476A CN110205681B CN 110205681 B CN110205681 B CN 110205681B CN 201910479476 A CN201910479476 A CN 201910479476A CN 110205681 B CN110205681 B CN 110205681B
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CN110205681A (en
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沈桂英
赵有文
孙静
刘京明
余丁
谢辉
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    • 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
    • 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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    • 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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    • G01—MEASURING; TESTING
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    • G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract

An indium arsenide single crystal wafer dislocation corrosion liquid and a dislocation corrosion detection method relate to the technical field of defect detection. The dislocation corrosive liquid for the indium arsenide single crystal chip mainly comprises hydrochloric acid, sulfuric acid and water. The dislocation corrosive liquid provided by the invention has the advantages of low price of raw materials, easiness in obtaining and high corrosion efficiency. The invention also provides a method for detecting dislocation corrosion by using the dislocation corrosion liquid, which comprises the following steps: and placing the indium arsenide single crystal wafer into a corrosive liquid, corroding to obtain the dislocation corroded indium arsenide single crystal wafer, cleaning the surface of the dislocation corroded indium arsenide single crystal wafer, and observing. The dislocation corrosion detection method provided by the invention is simple to operate and high in corrosion efficiency, and can quickly and clearly display the dislocation in the indium arsenide single crystal wafer.

Description

Dislocation corrosion liquid for indium arsenide single crystal wafer and dislocation corrosion detection method
Technical Field
The invention relates to the technical field of defect detection, in particular to an indium arsenide single crystal wafer dislocation corrosion liquid and a dislocation corrosion detection method.
Background
The infrared detector is one of the most core photoelectric devices of an infrared system, the infrared detection technology is in the key period from a second generation two-dimensional staring Focal Plane Array (FPA) area array imaging system to a third generation FPA imaging system at present, and the third generation system has the characteristics of large size, high pixel density, multi-wavelength detection and the like. The current commercial infrared detector material HgCdTe has the defects of poor crystal structure integrity, low working temperature, small substrate size and the like, so that the large-scale development and application of the material are limited. Compared with the InAs/GaSb II type superlattice material, the InAs/GaSb II type superlattice material has the advantages of low Auger recombination rate, long carrier service life, good material uniformity and the like, and becomes an ideal material for preparing large-scale focal plane arrays.
Indium arsenide is used as a source and a substrate material for manufacturing a novel infrared detector and a novel laser, high-density dislocation defects are easily generated in the crystal growth process, and stress is generated by taking the dislocation defects as a base point in the epitaxial growth process, so that the growth quality of an epitaxial film on the substrate is influenced. The dislocation density of single crystal materials has a critical effect on the performance of epitaxially grown devices, and thus it is necessary to conduct intensive research on dislocations in indium arsenide.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide an indium arsenide single crystal wafer dislocation etching solution and a dislocation etching detection method, so as to at least partially solve at least one of the above-mentioned technical problems.
As a first aspect of the invention, the invention provides an indium arsenide single crystal wafer dislocation etching solution which mainly comprises hydrochloric acid, sulfuric acid and water.
As a second aspect of the present invention, there is provided a method for detecting dislocation corrosion using the above dislocation corrosion liquid, comprising the steps of:
placing the indium arsenide single crystal wafer in a corrosive liquid for corrosion to obtain a dislocation-corroded indium arsenide single crystal wafer;
and cleaning the surface of the indium arsenide single crystal wafer after dislocation corrosion is completed, and then observing the indium arsenide single crystal wafer.
Compared with the prior art, the invention has the following beneficial effects:
(1) the dislocation corrosion solution provided by the invention has a better preferential corrosion effect on the indium arsenide single crystal wafer, and the raw materials are low in price, easy to obtain and high in corrosion efficiency.
(2) The dislocation corrosion detection method provided by the invention is simple to operate and high in corrosion efficiency, and can quickly and clearly display the dislocation in the indium arsenide single crystal wafer. The dislocation density of the indium arsenide single crystal grown by the liquid seal Czochralski technique was about 10 as detected by dislocation corrosion4cm-2The requirement for high quality of the substrate material can be satisfied.
Drawings
FIG. 1 is a flow chart of the dislocation corrosion detection method for an indium arsenide single crystal wafer according to the present invention;
FIG. 2 is a photograph showing the dislocation etched surface of an indium arsenide single crystal wafer in example 1 of the present invention;
FIG. 3 is a photograph showing the dislocation etched surface of an indium arsenide single crystal wafer in example 2 of the present invention;
FIG. 4 is a photograph showing the dislocation etched surface of the single crystal indium arsenide wafer in example 3;
FIG. 5 is a photograph showing the surface of an indium arsenide single crystal wafer according to comparative example 1 of the present invention after dislocation etching;
FIG. 6 is a photograph showing the surface of an indium arsenide single crystal wafer according to comparative example 2 of the present invention after dislocation etching.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention discloses an indium arsenide single crystal wafer dislocation corrosive liquid which mainly comprises hydrochloric acid, sulfuric acid and water.
The dislocation corrosive liquid provided by the invention has the advantages of low price of raw materials, easiness in obtaining and high corrosion efficiency.
Furthermore, the volume ratio of the hydrochloric acid to the sulfuric acid to the water in the corrosive liquid is (1-10) to (0-2) to (0-1) according to the volume fraction;
wherein, the mass concentration of the hydrochloric acid is 36-38%, and the mass concentration of the sulfuric acid is 70-98%.
Further, the indium arsenide single crystal wafer is an indium arsenide single crystal wafer having a {100} crystal orientation.
Further, the water is deionized water.
The invention also discloses a method for detecting dislocation corrosion by adopting the dislocation corrosion liquid, which comprises the following steps:
step A: placing the indium arsenide single crystal wafer in a corrosive liquid for corrosion to obtain a dislocation-corroded indium arsenide single crystal wafer;
and B: and cleaning the surface of the indium arsenide single crystal wafer subjected to dislocation corrosion, and observing the dislocation density of the indium arsenide single crystal wafer.
Further, the etching temperature is 10 to 50 ℃, preferably 20 ℃.
Further, the etching time is 1-20min, preferably 4 min.
Further, the specific operation of step B is: washing the indium arsenide single crystal wafer subjected to dislocation corrosion with water for 5-8 times, then drying the surface of the wafer with nitrogen, and detecting the dislocation density under a metallographic microscope;
preferably, the water is deionized water.
Further, the dislocation corrosion detection method further comprises the step of pretreating the indium arsenide single crystal before corrosion, and specifically comprises the following steps:
cleaning the polished indium arsenide single crystal wafer by using an organic solvent and water in sequence to remove surface contamination, and drying the wafer by using nitrogen after cleaning by using water for later use;
further, the organic solvent is acetone and/or absolute ethyl alcohol; the water is deionized water.
The technical solution of the present invention is further illustrated by the following specific embodiments in conjunction with the accompanying drawings. It should be noted that the following specific examples are given by way of illustration only and the scope of the present invention is not limited thereto.
The chemicals and raw materials used in the following examples were either commercially available or self-prepared by a known preparation method.
Example 1
A {100} indium arsenide single crystal chip dislocation corrosion detection corrosion method, the corrosive liquid is composed of analytically pure AR grade hydrochloric acid, analytically pure AR grade sulfuric acid and deionized water, the volume ratio is 1: 2: 1;
wherein, the mass concentration of the hydrochloric acid is 36.5 percent, and the mass concentration of the sulfuric acid is 96 percent.
The method for detecting dislocation corrosion of the polished indium arsenide single crystal wafer with the {100} crystal orientation by adopting the etching solution comprises the following steps:
(1) preparing dislocation corrosive liquid by adopting hydrochloric acid, sulfuric acid and deionized water at room temperature, and continuously stirring in the preparation process to fully mix the solution;
(2) cleaning the polished indium arsenide single crystal wafer by using acetone, absolute ethyl alcohol and deionized water in sequence to remove surface stains, and blowing the wafer to be reserved by using nitrogen after the wafer is washed by the deionized water;
(3) placing the dried indium arsenide single crystal wafer into a dry basket, slowly placing the dried indium arsenide single crystal wafer into prepared corrosive liquid, and corroding for 3 min;
(4) and rapidly taking out the indium arsenide single crystal wafer subjected to dislocation corrosion, washing the indium arsenide single crystal wafer for 5-8 times by using deionized water, blow-drying the surface of the wafer by using nitrogen, and detecting the dislocation density under a metallographic microscope.
In this example, when the dislocation-etched indium arsenide single crystal wafer is placed under a metallographic microscope and magnified 200 times, a picture as shown in fig. 2 is observed, and a significant etch pit is observed. Statistically, the dislocation density is about 10120/cm2。
Example 2
A {100} indium arsenide single crystal chip dislocation corrosion detection corrosion method, the corrosive liquid is composed of analytically pure AR grade hydrochloric acid, analytically pure AR grade sulfuric acid and deionized water, the volume ratio is 2: 1;
wherein, the mass concentration of the hydrochloric acid is 36.5 percent, and the mass concentration of the sulfuric acid is 96 percent.
The method for detecting dislocation corrosion of the polished indium arsenide single crystal wafer with the {100} crystal orientation by adopting the etching solution comprises the following steps:
(1) preparing dislocation corrosive liquid by adopting hydrochloric acid, sulfuric acid and deionized water at room temperature, and continuously stirring in the preparation process to fully mix the solution;
(2) cleaning the polished indium arsenide single crystal wafer by using acetone, absolute ethyl alcohol and deionized water in sequence to remove surface stains, and blowing the wafer to be reserved by using nitrogen after the wafer is washed by the deionized water;
(3) placing the dried indium arsenide single crystal wafer into a dry basket, slowly placing the dried indium arsenide single crystal wafer into prepared corrosive liquid, and corroding for 2 min;
(4) and rapidly taking out the indium arsenide single crystal wafer subjected to dislocation corrosion, washing the indium arsenide single crystal wafer for 5-8 times by using deionized water, blow-drying the surface of the wafer by using nitrogen, and detecting the dislocation density under a metallographic microscope.
In this example, when the dislocation-etched indium arsenide single crystal wafer is placed under a metallographic microscope and magnified 200 times, a picture as shown in fig. 3 is observed, and a significant etch pit is observed. Statistically, the dislocation density is about 98765 dislocations/cm2。
Example 3
The content of the embodiment is basically the same as that of the embodiment 1, except that the corrosive liquid consists of analytically pure AR-grade hydrochloric acid and deionized water, and the volume ratio is 10: 1;
wherein the mass concentration of the hydrochloric acid is 36.5 percent.
The method for detecting dislocation corrosion of the polished indium arsenide single crystal wafer with the {100} crystal orientation by adopting the etching solution comprises the following steps:
(1) preparing dislocation corrosive liquid by adopting hydrochloric acid and deionized water at room temperature, and continuously stirring in the preparation process to fully mix the solution;
(2) cleaning the polished indium arsenide single crystal wafer by using acetone, absolute ethyl alcohol and deionized water in sequence to remove surface stains, and blowing the wafer to be reserved by using nitrogen after the wafer is washed by the deionized water;
(3) placing the dried indium arsenide single crystal wafer into a dry basket, slowly placing the dried indium arsenide single crystal wafer into prepared corrosive liquid, and corroding for 4 min;
(4) and rapidly taking out the indium arsenide single crystal wafer subjected to dislocation corrosion, washing the indium arsenide single crystal wafer for 5-8 times by using deionized water, blow-drying the surface of the wafer by using nitrogen, and detecting the dislocation density under a metallographic microscope.
In this example, when the dislocation-etched indium arsenide single crystal wafer is placed under a metallographic microscope and magnified 200 times, a picture as shown in fig. 4 can be observed, and a significant etch pit can be seen in the picture. Statistically, the dislocation density is approximately 11865 dislocations/cm2。
The dislocation etching pictures in the embodiments 1 to 3 are shown in fig. 2 to 4, and the method for etching the {100} crystal orientation indium arsenide single crystal wafer is successfully obtained according to the basic principle of preferential etching by combining theory and practice.
Comparative example 1
As a comparative example, an etching solution composed of nitric acid, hydrofluoric acid and deionized water was prepared in a volume ratio of 2: 1;
wherein the mass concentration of the nitric acid is 65 percent, and the mass concentration of the hydrofluoric acid is 40 percent.
The dislocation corrosion experiment of the indium arsenide single crystal wafer with the {100} crystal orientation after polishing is carried out by adopting the etching solution, and the dislocation corrosion experiment comprises the following steps:
(1) preparing dislocation corrosive liquid by using nitric acid, hydrofluoric acid and deionized water at room temperature, wherein continuous stirring is required in the preparation process to fully mix the solution;
(2) cleaning the polished indium arsenide single crystal wafer by using acetone, absolute ethyl alcohol and deionized water in sequence to remove surface stains, and blowing the wafer to be reserved by using nitrogen after the wafer is washed by the deionized water;
(3) placing the dried indium arsenide single crystal wafer into a dry basket, slowly placing the dried indium arsenide single crystal wafer into prepared corrosive liquid, and corroding for 2 min;
(4) and rapidly taking out the dislocation corrosion-finished indium arsenide single crystal wafer, washing the wafer for 5-8 times by using deionized water, blow-drying the surface of the wafer by using nitrogen, and observing the surface of the wafer under a metallographic microscope.
In this example, when the etched indium arsenide single crystal wafer is placed under a metallographic microscope and magnified by 100 times, a picture as shown in fig. 5 can be observed, in which pits having different sizes and different orientations are visible, and the shapes and orientations of the pits do not conform to the basic rule of the alignment of dislocation pits, so that the pits are not dislocation pits. Therefore, an etching solution composed of nitric acid, hydrofluoric acid and deionized water is not an effective etchant for etching a {100} crystal orientation indium arsenide single crystal.
Comparative example 2
As a comparative example, an etching solution consisting of nitric acid, hydrochloric acid and deionized water is prepared, and the volume ratio is 2: 1;
wherein the mass concentration of the nitric acid is 65 percent, and the mass concentration of the hydrochloric acid is 36.5 percent.
The dislocation corrosion experiment of the indium arsenide single crystal wafer with the {100} crystal orientation after polishing is carried out by adopting the etching solution, and the dislocation corrosion experiment comprises the following steps:
(1) preparing dislocation corrosive liquid by using nitric acid, hydrochloric acid and deionized water at room temperature, wherein continuous stirring is required in the preparation process to fully mix the solution;
(2) cleaning the polished indium arsenide single crystal wafer by using acetone, absolute ethyl alcohol and deionized water in sequence to remove surface stains, and blowing the wafer to be reserved by using nitrogen after the wafer is washed by the deionized water;
(3) placing the dried indium arsenide single crystal wafer into a dry basket, slowly placing the dried indium arsenide single crystal wafer into prepared corrosive liquid, and corroding for 2 min;
(4) and rapidly taking out the dislocation corrosion-finished indium arsenide single crystal wafer, washing the wafer for 5-8 times by using deionized water, blow-drying the surface of the wafer by using nitrogen, and observing the surface of the wafer under a metallographic microscope.
In this comparative example, the dislocation-etched indium arsenide single crystal wafer was placed under a metallographic microscope and magnified 100 times, and a picture as shown in fig. 6 was observed, in which circular ring-shaped shallow pits with different sizes were observed, and the pits were different in size and blurred in boundary and were not dislocation pits. Therefore, the etching solution composed of nitric acid, hydrochloric acid and deionized water is not an effective etchant for etching the {100} crystal orientation indium arsenide single crystal.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The application of the indium arsenide single crystal wafer dislocation corrosion liquid in the dislocation corrosion detection of the indium arsenide single crystal wafer is characterized in that the indium arsenide single crystal wafer dislocation corrosion liquid consists of hydrochloric acid, sulfuric acid and water, and the volume ratio is 1: 2: 1 or 2: 1; alternatively, the first and second electrodes may be,
the indium arsenide single crystal wafer dislocation corrosion liquid consists of hydrochloric acid and water, and the volume ratio is 10: 1;
the indium arsenide single crystal wafer is an indium arsenide single crystal wafer with a {100} crystal orientation;
wherein the mass concentration of the hydrochloric acid is 36-38%, and the mass concentration of the sulfuric acid is 96-98%.
2. The application of the indium arsenide single crystal wafer dislocation corrosion liquid in the detection of the dislocation corrosion of the indium arsenide single crystal wafer as claimed in claim 1, wherein the water is deionized water.
3. A method for detecting dislocation corrosion by using the dislocation corrosion solution of the indium arsenide single crystal wafer as claimed in any of claims 1-2, comprising the steps of:
placing the indium arsenide single crystal wafer in a corrosive liquid for corrosion to obtain a dislocation-corroded indium arsenide single crystal wafer;
cleaning the surface of the indium arsenide single crystal wafer after dislocation corrosion is completed, and then observing the indium arsenide single crystal wafer;
wherein the indium arsenide single crystal wafer is an indium arsenide single crystal wafer with a {100} crystal orientation.
4. A dislocation corrosion detection method according to claim 3, characterized in that the corrosion temperature is 10-50 ℃.
5. Dislocation corrosion detection method according to claim 4, characterized in that said corrosion temperature is 20 ℃.
6. A dislocation corrosion detection method according to claim 3, characterized in that the corrosion time is 1-20 min.
7. Dislocation corrosion detection method according to claim 6, characterized in that said corrosion time is 4 min.
8. A dislocation corrosion detection method as claimed in claim 3, wherein said step of cleaning the surface comprises: washing the dislocation corroded indium arsenide single crystal wafer for 5-8 times by using water, and then drying the surface of the wafer by using nitrogen;
the step of observing comprises: detecting the dislocation density of the indium arsenide single crystal wafer under a metallographic microscope;
the water is deionized water.
9. The dislocation corrosion detection method according to claim 3, further comprising a step of pretreating the indium arsenide single crystal wafer before etching, the step of pretreating comprising:
and cleaning the polished indium arsenide single crystal wafer by using an organic solvent and water in sequence to remove surface contamination, and drying the wafer by using nitrogen after cleaning by using water for later use.
10. Dislocation corrosion detection method according to claim 9, characterized in that said organic solvent is acetone and/or absolute ethanol; the water is deionized water.
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