WO2013074330A1 - Etching agent for type ii inas/galnsb superlattice epitaxial materials - Google Patents

Etching agent for type ii inas/galnsb superlattice epitaxial materials Download PDF

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WO2013074330A1
WO2013074330A1 PCT/US2012/063700 US2012063700W WO2013074330A1 WO 2013074330 A1 WO2013074330 A1 WO 2013074330A1 US 2012063700 W US2012063700 W US 2012063700W WO 2013074330 A1 WO2013074330 A1 WO 2013074330A1
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inas
galnsb
etching
solution
type
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Edward H AIFER
Sergey I MAXIMENKO
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US Department of Navy
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P90/00—Preparation of wafers not covered by a single main group of this subclass, e.g. wafer reinforcement
    • H10P90/12—Preparing bulk and homogeneous wafers
    • 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

Definitions

  • the disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in a Type II superlattice matched to (100) GaSb.
  • One aspect of this disclosure involves a method for revealing crystallographic defects on the (100) face of Type II InAs/GalnSb based superlattice structures by preferential wet chemical etching.
  • T2SLs Type II InAs/Gai-xhixSb superlattices (T2SLs) lattice matched to GaSb substrates (x typically ⁇ 20%) are an important semiconductor hetero structure material systems for applications in mid-, long- and very long-wave infrared detectors. They have theoretical performance limits well beyond those of incumbent technologies based on InSb and HgCdTe.
  • T2SLs were first introduced in the 1970s by Sai-Halasz, Tsu and Esaki, and then a decade later, were proposed by Smith and Mailhiot to be used for infrared detection.
  • state- of-the-art T2SL material is grown using molecular beam epitaxy (MBE) on (100) GaSb substrates.
  • MBE molecular beam epitaxy
  • the period structure of the basic binary form of T2SL consists of a pair of 1 to 5 nm-thick
  • the ternary T2SL is an alternate form in which GaSb is replaced by Ga(l-x)In(x)Sb in the superlattice, and strain is balanced by adjusting the InSb-alloy fraction "x" in the ternary layer and dispensing with the half-ML of InSb at each interface.
  • T2SLs may be readily doped n- or /?-type, and have been used to construct an enormous variety of infrared sensor structures, with epitaxial thicknesses of up to -15 ⁇ ' ⁇ .
  • T2SL technology has not yet achieved its full theoretical promise, largely due to the presence of bulk and surface crystallographic defects generated during MBE growth and device fabrication that promote excess dark current.
  • defect structures are identified by subjecting the material to a wet chemical etch that has the characteristic of being amplified in the presence of crystallographic defects, and then analyzing the density, location and physical structure of resulting etch pits.
  • etch pit defect delineation in (100) GaSb for example, a two-step etch process was used by J. Doershel, and U. Geissler where the surface was first chemically polished in a 2: 18:40 (volume ratio) solution of HF:HN0 3 :CH 3 COOH, followed by etching in 2: 1 solution of HC1:H 2 0 2 . Constant vigorous agitation was necessary to obtain reliable results.
  • Costa et al. used a (5: 1) solution of H 2 S0 4 :H 2 0 2 as well as (5: 1) Cr0 3 (5 M aqua, solution. ):HF for etch pit delineation on GaSb (100).
  • Yonenaga employed a 2.4x10 " molar solution of AgN0 3 in (3:2:5) HN0 3 :HF:H 2 0.
  • This disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb.
  • Figure 1 illustrates GaSb, InAs (F-43m space group), Zinc-Blende Lattice.
  • Figure 2 illustrates etch pits from inclusion and etch pits from dislocations in the film.
  • Figure 3 illustrates typical etch pits in type II TSL.
  • Figure 4 illustrates chemical etching results of raw wafers. Rectangular etch pits with well-defined crystallographic facets form in locations containing dislocations in the crystal structure.
  • Figure 5 illustrates correlation between electrically active defects, leakage current and etch pits. Shown are electrically active defects (dark spots) presented in devices with increased leakage current. Also shown is one to one correlation between electrically active defects mapped by EBIC and etch pits.
  • This disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb.
  • the etching agent comprises a (2.5:4.5: 16.5:280) solution by volume or (1%:2%:9%:88%) by weight, of HF:H 2 0 2 :H 2 S0 4 :H 2 0.
  • the etchant is made by mixing (49%) hydrofluoric aqueous solution with (30%) water-based peroxide, followed by sulfuric acid, and diluted with de-ionized H20 (D I- water). Etching can be carried out at room temperature (around 20° C), without stirring.
  • Typical etching times for the (100) face of a T2SL are in the range of 60-90 seconds.
  • the samples are rinsed thoroughly in DI- water and then dried using N 2 gas.
  • the morphology of the etch pits and surface may be varied by adjusting the ratios of the etching solution from the mixture given above. For example, increasing the HF or H 2 0 2 content leads to a more isotropic etch, with rounded etch pits. Increasing H 2 S0 4 or decreasing HF content introduces more anisotropic etching of the surface. In addition, increasing H 2 S0 4 or decreasing HF introduces nonuniform etching of the surface, making reliable identification of defects difficult.
  • Etching time is controlled by dilution with water, and for a typical long-wave infrared T2SL etched in the above solution with 88% DI- water by weight, etch pits ranging from 4-20 ⁇ in diameter are formed after 60-90 seconds. Etch pits of this size are readily observed using optical differential interference contrast (Nomarski) microscopy.
  • this novel etchant on T2SLs enables the detection and identification of various imperfections in the crystalline structure of the material, as etch pit formation is promoted and governed by the structure of the underlying defect.
  • threading dislocations are indicated by large, deep rectangular pits, having bottom point symmetries reflecting dislocation direction.
  • Misfit dislocations half-loop arrays
  • twin shallow rectangular etch pits indicating the termination points of the half loops at the surface. More rounded, flat bottomed pits correspond to agglomerations of impurities.
  • the etch produces linear striations aligned along -U anc j [1 10]directions in the presence of stacking faults in 1) and ⁇ glide planes.
  • etch-pit structure the structure of the underlying crystallographic defect, and the activity level of the defect with respect to dark current, were studied using electron beam induced current (EBIC) mapping of defects and cross-sectional transmission electron microscopy (TEM) to reveal the defect structure.
  • EBIC electron beam induced current
  • TEM cross-sectional transmission electron microscopy
  • etch pit definition was marginal however as the increased water content also heavily degraded the shape of the etch pits as the etch became more isotropic. As a result, dilution was limited to a level with etching times of only 10-20 seconds, making control of the etching process difficult. Constant vigorous agitation of the etch bath was also necessary to remove gaseous products nucleated on the sample surface.
  • the etching agent can comprise a (2.5:4.5: 16.5:280) solution by volume or (1%:2%:9%:88%) by weight, of HF:H 2 0 2 :H 2 S0 4 :H 2 0 and, as discussed, variations are possible.
  • the above description is that of a preferred embodiment of the invention. Various modifications and variations are possible in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described. Any reference to claim elements in the singular, e.g., using the articles "a,” “an,” “the,” or “said” is not construed as limiting the element to the singular.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)
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  • Testing Or Measuring Of Semiconductors Or The Like (AREA)

Abstract

This disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb. The etching agent comprises a (2.5:4.5:16.5:280) solution by volume or (1%:2%:9%:88%) by weight, of HF:H2O2:H2SO4:H2O. The etchant is made by mixing (49%) hydrofluoric aqueous solution with (30%) water-based peroxide, followed by sulfuric acid, and diluted with de-ionized H20 (DI-water).

Description

TITLE OF THE INVENTION
Etching Agent for Type II InAs/GalnSb Superlattice Epitaxial Materials CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a non-provisional application of and claims priority to and benefits of United States Patent Application Number 61/559,430 filed 11/14/2011.
BACKGROUND OF THE INVENTION
(1) Technical Field of the Invention
The disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in a Type II superlattice matched to (100) GaSb.
(2) Description of Related Art
One aspect of this disclosure involves a method for revealing crystallographic defects on the (100) face of Type II InAs/GalnSb based superlattice structures by preferential wet chemical etching.
Type II InAs/Gai-xhixSb superlattices (T2SLs) lattice matched to GaSb substrates (x typically < 20%) are an important semiconductor hetero structure material systems for applications in mid-, long- and very long-wave infrared detectors. They have theoretical performance limits well beyond those of incumbent technologies based on InSb and HgCdTe.
T2SLs were first introduced in the 1970s by Sai-Halasz, Tsu and Esaki, and then a decade later, were proposed by Smith and Mailhiot to be used for infrared detection. Presently, state- of-the-art T2SL material is grown using molecular beam epitaxy (MBE) on (100) GaSb substrates.
The period structure of the basic binary form of T2SL consists of a pair of 1 to 5 nm-thick
InAs and GaSb layers. Approximately one additional monolayer (ML) of InSb (a = 6.4794A) is also required in each period to balance the strain with respect to the GaSb substrate (a =
6.0959A) resulting from the shorter lattice constant of InAs (a = 6.0583A). The ternary T2SL is an alternate form in which GaSb is replaced by Ga(l-x)In(x)Sb in the superlattice, and strain is balanced by adjusting the InSb-alloy fraction "x" in the ternary layer and dispensing with the half-ML of InSb at each interface. These and several other types of T2SLs may be readily doped n- or /?-type, and have been used to construct an enormous variety of infrared sensor structures, with epitaxial thicknesses of up to -15 μηι'β.
Despite more than 30 years of study, however, T2SL technology has not yet achieved its full theoretical promise, largely due to the presence of bulk and surface crystallographic defects generated during MBE growth and device fabrication that promote excess dark current.
Progress in understanding the nature of these defects and how to remediate them has been hindered by the difficulty in identifying specific defect structures in this material system.
One widely used technique that has been used successfully to identify defects with densities of up to -10 5 cm -"2 on substrates and epitaxial material, is preferential chemical etching. Here, defect structures are identified by subjecting the material to a wet chemical etch that has the characteristic of being amplified in the presence of crystallographic defects, and then analyzing the density, location and physical structure of resulting etch pits.
Though a number of techniques exist to preferentially etch GaSb and InAs on different crystallographic planes, no such techniques have heretofore existed for superlattices composed of periodic combinations of thin layers of these materials. This is due to the fact that though InAs and GalnSb belong to the same -43m point symmetry group, the difference in chemical composition yields a large contrast in preferential etch rates of these materials.
For etch pit defect delineation in (100) GaSb for example, a two-step etch process was used by J. Doershel, and U. Geissler where the surface was first chemically polished in a 2: 18:40 (volume ratio) solution of HF:HN03:CH3COOH, followed by etching in 2: 1 solution of HC1:H202. Constant vigorous agitation was necessary to obtain reliable results.
Costa et al. used a (5: 1) solution of H2S04:H202 as well as (5: 1) Cr03 (5 M aqua, solution. ):HF for etch pit delineation on GaSb (100). For preferential etching of InAs (111) orientation, Yonenaga employed a 2.4x10" molar solution of AgN03 in (3:2:5) HN03:HF:H20.
We have found no previously published data, however, on preferential etching of InAs/GalnSb superlattices, indicating the lack of a common etching solution with similar preferential etch rates for both compound materials. Thus we submit this disclosure of a single etchant which reveals and distinguishes crystallographic defects on (100) T2SLs through etch pit structures defined by preferential wet chemical etching.
DISCLOSURE OF THE INVENTION
This disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 illustrates GaSb, InAs (F-43m space group), Zinc-Blende Lattice.
Figure 2 illustrates etch pits from inclusion and etch pits from dislocations in the film.
Figure 3 illustrates typical etch pits in type II TSL.
Figure 4 illustrates chemical etching results of raw wafers. Rectangular etch pits with well-defined crystallographic facets form in locations containing dislocations in the crystal structure.
Figure 5 illustrates correlation between electrically active defects, leakage current and etch pits. Shown are electrically active defects (dark spots) presented in devices with increased leakage current. Also shown is one to one correlation between electrically active defects mapped by EBIC and etch pits.
BEST MODES FOR CARRYING OUT THE INVENTION
This disclosure involves a formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb.
The etching agent comprises a (2.5:4.5: 16.5:280) solution by volume or (1%:2%:9%:88%) by weight, of HF:H202:H2S04:H20.
The etchant is made by mixing (49%) hydrofluoric aqueous solution with (30%) water-based peroxide, followed by sulfuric acid, and diluted with de-ionized H20 (D I- water). Etching can be carried out at room temperature (around 20° C), without stirring.
Typical etching times for the (100) face of a T2SL are in the range of 60-90 seconds.
After etching, the samples are rinsed thoroughly in DI- water and then dried using N2 gas.
Under these conditions, using a freshly prepared solution, rectangular etch pits with well- defined crystallographic facets form in locations containing dislocations in the crystal structure. The resulting etch pits are oriented with the longest axis aligned along the [0 1 1] crystallographic direction.
The morphology of the etch pits and surface may be varied by adjusting the ratios of the etching solution from the mixture given above. For example, increasing the HF or H202 content leads to a more isotropic etch, with rounded etch pits. Increasing H2S04 or decreasing HF content introduces more anisotropic etching of the surface. In addition, increasing H2S04 or decreasing HF introduces nonuniform etching of the surface, making reliable identification of defects difficult.
Etching time is controlled by dilution with water, and for a typical long-wave infrared T2SL etched in the above solution with 88% DI- water by weight, etch pits ranging from 4-20 μιη in diameter are formed after 60-90 seconds. Etch pits of this size are readily observed using optical differential interference contrast (Nomarski) microscopy.
The application of this novel etchant on T2SLs enables the detection and identification of various imperfections in the crystalline structure of the material, as etch pit formation is promoted and governed by the structure of the underlying defect.
For example, threading dislocations are indicated by large, deep rectangular pits, having bottom point symmetries reflecting dislocation direction. Misfit dislocations (half-loop arrays) are marked by twin shallow rectangular etch pits indicating the termination points of the half loops at the surface. More rounded, flat bottomed pits correspond to agglomerations of impurities.
In addition, the etch produces linear striations aligned along -U ancj [1 10]directions in the presence of stacking faults in 1) and ^ glide planes. The correlation between etch-pit structure, the structure of the underlying crystallographic defect, and the activity level of the defect with respect to dark current, were studied using electron beam induced current (EBIC) mapping of defects and cross-sectional transmission electron microscopy (TEM) to reveal the defect structure. TEM and EBIC confirmed strong correspondence between etch pit and crystallographic defect structure. We found no other published data showing successful preferential etching of InAs/GalnSb superlattices, though a mixture of HF:H202:H2S04:H20 has been reported for preferential etching of dislocations on GaAsxPi semiconductors where x is in the range of 0 to 1 and consisted of HF:H202:H2S04:H20 (6-18 :6-20 :20-55 :30-55 ) by weight. We tested several etchants suggested for preferential etching of GaSb and InAs, including a modified two-step etch process of Doershel et al. consisting of an initial polish in HF:HN03:CH3COOH (2: 18:40) followed by etch-pit delineation in HC1: H202 (2: 1).
Upon testing, it was found that this procedure generally produced a highly non-uniform surface against which etched features were difficult to discern. The best performance was achieved by diluting the polishing etch as HF:HN03:CH3COOH:H20 (2: 18:40:30) by volume, and eliminating the second etch step HC1: H202 (2: 1) entirely.
While dilution lowered the etch rate improving control, etch pit definition was marginal however as the increased water content also heavily degraded the shape of the etch pits as the etch became more isotropic. As a result, dilution was limited to a level with etching times of only 10-20 seconds, making control of the etching process difficult. Constant vigorous agitation of the etch bath was also necessary to remove gaseous products nucleated on the sample surface.
As such, our discovery overcame such problems and produced the best results. Our formula, mixing procedure, etching technique and application of an etchant for revealing defects in T2SL's grown lattice matched to (100) GaSb are herein disclosed. The etching agent can comprise a (2.5:4.5: 16.5:280) solution by volume or (1%:2%:9%:88%) by weight, of HF:H202:H2S04:H20 and, as discussed, variations are possible. The above description is that of a preferred embodiment of the invention. Various modifications and variations are possible in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described. Any reference to claim elements in the singular, e.g., using the articles "a," "an," "the," or "said" is not construed as limiting the element to the singular.

Claims

Claims What we claim is:
1. An etchant comprising: a (2.5:4.5: 16.5:280) solution by volume of HF:H202:H2S04:H20.
2. A solution for etching type II InAs/GalnSb superlattice epitaxial materials comprising: a (1%:2%:9%:88%) solution by weight HF:H202:H2S04:H20.
3. A method of making a solution for etching type II InAs/GalnSb superlattice epitaxial materials comprising: mixing a hydrofluoric aqueous solution with a water-based peroxide to form a first solution; mixing the first solution with sulfuric acid to form a second solution; and diluting the second solution with de-ionized water.
4. The method of making of claim 3 wherein the hydrofluoric aqueous solution is a 49% by weight hydrofluoric aqueous solution and wherein the water-based peroxide is a 30% by weight water-based peroxide.
5. A method of etching type II InAs/GalnSb superlattice epitaxial materials comprising: forming an etchant comprising a (2.5:4.5: 16.5:280) solution by volume of HF:H202:H2S04:H20; applying the etchant to a type II InAs/GalnSb superlattice epitaxial material; conducting the step of applying the etchant to a type II InAs/GalnSb superlattice epitaxial material at a temperature of about 20 degrees C; and controlling the etching time by diluting with water.
6. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 5 wherein the etching is conducted for about 60 to about 90 seconds and results in etch pits of about 4 to about 20 μιη in diameter.
7. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 6 wherein the etching does not involve stirring.
8. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 7 wherein there is no surface treatment before etching.
9. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 6 further including rinsing in deionized water; and drying using nitrogen gas.
10. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 6 further including forming rectangular etch pits with crystollagraphic facets in locations containing dislocations in the crystal structure.
11. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 10 wherein the resulting etch pits are oriented with the longest axis aligned along the [O i l ] crystallographic direction.
12. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 6 further including forming increasing the HF or Η202 and producing an isotropic etch with rounded etch pits with crystoUagraphic facets in locations containing dislocations in the crystal structure.
13. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 6 further including forming etch pits with crystoUagraphic facets in locations containing dislocations in the crystal structure; and correlating the shape of the etch pit to the type of dislocation or impurity.
14. The method of etching type II InAs/GalnSb superlattice epitaxial materials of claim 13 wherein a rectangular pit having bottom point symmetries reflecting dislocation direction correlates to threading dislocations and wherein twin rectangular etch pits are correlated to misfit dislocations with half loop termination points.
PCT/US2012/063700 2011-11-14 2012-11-06 Etching agent for type ii inas/galnsb superlattice epitaxial materials Ceased WO2013074330A1 (en)

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US61/559,430 2011-11-14

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JP6510265B2 (en) * 2015-02-23 2019-05-08 旭化成エレクトロニクス株式会社 Method for manufacturing quantum infrared device and etchant for manufacturing quantum infrared device
CN110205681B (en) * 2019-06-03 2020-12-15 中国科学院半导体研究所 Indium arsenide single wafer dislocation etching solution and dislocation etching detection method
CN115992390B (en) * 2023-01-09 2023-05-26 苏州焜原光电有限公司 Surface treatment method for molecular beam epitaxial gallium antimonide substrate
CN117286501A (en) * 2023-09-21 2023-12-26 安徽光智科技有限公司 GaSb substrate etching solution and etching method on InAsSb chip and InAsSb chip

Citations (2)

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US4459216A (en) * 1982-05-08 1984-07-10 Mitsubishi Gas Chemical Company, Inc. Chemical dissolving solution for metals
US20060086372A1 (en) * 2002-06-22 2006-04-27 Raimund Mellies Composition for the removing of sidewall residues

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Publication number Priority date Publication date Assignee Title
DE2638302A1 (en) 1976-08-25 1978-03-02 Wacker Chemitronic DETERGENT FOR III / V SEMICONDUCTORS

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4459216A (en) * 1982-05-08 1984-07-10 Mitsubishi Gas Chemical Company, Inc. Chemical dissolving solution for metals
US20060086372A1 (en) * 2002-06-22 2006-04-27 Raimund Mellies Composition for the removing of sidewall residues

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