Guide To References On III–V Semiconductor Chemical Etching
Materials Science and Engineering, 31 (2001) 1 438Guide to references on III V semiconductor chemical etchingA.R. Clawson*Department of Electrical and Computer Engineering, University of California at San Diego, 9500 Gilman Drive, La Jolla,CA 92093-0407, USAAccepted 27 August 2000AbstractThe literature on chemical etching of III V semiconductors is reviewed with the intent to organize citations incategories useful to device and materials investigators. Descriptive citations are grouped by the intended etchapplication and subgrouped by specific semiconductors for both wet and dry etching. A separate section groupscitations by the various chemical compositions used as etchants so that a broad view of results and issues can beaccessed. The final section lists references by author, with complete titles and notes of their relevance to etching.# 2001 Elsevier Science B.V. All rights reserved.Keywords: Chemical etching; Wet etchants; Dry etchants1. IntroductionThere is a large extent of literature on etchants, but it is frequently hard to locate specificinformation. The purpose of this reference guide is to direct the III V semiconductor deviceresearcher to chemical etchants suitable for particular applications and provide descriptions anduseful results. There are many excellent reviews of etchants that provide background for understanding the chemistry, and which give limited lists of applicable etchants with references. Thereare also many investigations characterizing specific etchants in detail. Other etchants are simplydescribed as a side issue to their application in device fabrication or materials characterization. Thereferences compiled here give a very broad sampling of what is available up to April 2000.This guide is given as four annotated sections to make the etching information as accessible aspossible. Section 2 lists wet etchants by there applications, Section 3 lists dry etchants by theirapplication, Section 4 lists the wet chemical etchants by chemical composition, and the last part is alist of the references, providing both titles and notation of the contents to establish the context of theetchant data.The wet etchant application categories in Section 2 are grouped into common themes. Notes ondifferent etchants are given, however, no judgement is made about the significance of the data. Someinformation is valuable and some is trivial, yet may give insight into device fabrication. Citations toreferences in the last part are indicated by first author's name and year with postscripts a, b, c, etc.when multiple references occur for a particular year.*Tel.: 1-858-534-7919.E-mail address: dawson@ece.ucsd.edu (A.R. Clawson).0927-796X/01/ see front matter # 2001 Elsevier Science B.V. All rights reserved.PII: S 0 9 2 7 - 7 9 6 X ( 0 0 ) 0 0 0 2 7 - 9
2A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438The dry etchant application categories in Section 3 are grouped into common themes. As withSection 2, citations to references in the last part are indicated by first author's name and year withpostscripts a, b, c, etc. when multiple references occur for a particular year.The wet chemical etchant list in Section 4 is ordered alphabetically by chemical, however,reference notes are grouped under only one arbitrarily chosen component of multi-componentetchants. Other commutations of the components are included to direct the reader to the appropriatelisting. H2O is usually not considered as a designated chemical component in the list, thus in mostcases dilute and concentrated etchants are grouped together.The etchant reference list of the last part is ordered alphabetically by first author. Completetitles and notes are given. The notes include data on materials, etch rates and specific etch conditionswhen possible.Hopefully this guide will help lead to the appropriate literature for detailed information.2. Wet etch applications2.1. Wet chemical etching reviewsReview of wet chemical etching of III Vs, covering electrochemical mechanisms of etching andpractical application of etchants; material selective etchants, defect revealing etchants, profileetching; Ref. (Notten, P.H.L., 1993)III V semiconductor etchant review: gives pre-1962 data on chemical etchants for InSb, GaSb, AlSb,InAs, GaAs, InP, GaP; Ref. (Faust, J.W., 1962)Review: general discussion of etch pit dislocation and hillock formation; Ref. (Faust, J.W., 1959)Review of electrochemical behavior of semiconductor electrodes; Ref. (Gerischer, H., 1959)Treatise on photochemical behavior of semiconductors; discusses thermodynamics and kinetics ofphotodecomposition and function of electrolyte junction solar cells; Ref. (Gerischer, H., 1979)Review: silicon defect etch pit delineation; Ref. (Heimann, R.B., 1982)Review of III V etching; describes mechanisms for (1) anodic (electrochemical) etching; (2)electroless etching (redox potential driven and illumination driven); (3) chemical etching; Ref.(Kelly, J.J., 1988)Review of Si and Ge etching; GaAs etching, GaAs electrochemical etching, GaAs thermochemicaletching; GaP etching; Ref. (Kern, W., 1978a)Review: chemical etching of insulators, semiconductors, and conductors; describes etchingprinciples and techniques; provides tables of etchants for GaAs, GaP, AlN, BN, BP, AlSb, GaN,GaSb, InAs, InP, InSb; Ref. (Kern, W., 1978b)Photochemical etching review: p n dopant selectivity; surface relief etching; InGaAsP/InP andGaAs; Ref. (Kohl, P.A., 1989)
A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438Treatise on photoelectrochemistry of semiconductor surfaces; Ref. (Pleskov, Yu.V., 1986)Review of GaAs etchant types, defect types, and defect revealing etchants; Ref. (Stirland, D.J., 1976)Review of etching behavior; gives definitions:Preferential Ð anisotropic etchants show markedly different etch rates on different low indexcrystallographic planesNon-preferential Ð etchants show etch rate independent of orientationSelective Ð etchants show markedly different etch rates for different semiconductor compositionsNon-selective Ð etchants show etch rates independent of composition; Ref. (Tijburg, R., 1976a)Review of semiconductor etching; discusses chemical process, effect of illumination, effect ofadding metal ions, and crystallographic effects. Gives tables of etchants for Si, Ge, SiC, GaAs, GaP,GaSb, InAs, InP, InSb, ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, PbS; Ref. (Tuck, B., 1975)Review: InP etching overview; wet chemical and dry etching; Ref. (Adachi, S., 1990a)Review: GaAs etching overview; wet and dry etching; Ref. (Ashby, C.I.H., 1990a)Review: InP wet chemical etching; with (1) defect or damage revealing etchant table, (2) polishingetchant table, and (3) pattern etchant table; Ref. (Adachi, S., 1990b)Review: wet and dry chemical etching of GaAs; classifies wet etchants as non-electrolyte (those withrates which are diffusion limited or chemical reaction limited) and electrolyte (those based on anodicoxidation followed by dissolution of products); gives tables of wet and dry etchants; Ref. (Ashby,C.I.H., 1990f)Review of GaAs etching and surface preparation; discusses etching mechanisms, diffusionand reaction rate limiting etching, anodic etching, and surface preparation; Ref. (Mukherjee, S.D.,1985)Review: photochemical processing of semiconductors; Ref. (Rauth, D.R., 1992)Review: chemical etching principles: dissolution of ionic crystals; dissolution of semiconductors;etch pit formation; electrochemical etching; photoetching; gas phase etching; Ref. (Sangwal, K.,1992)Review: STM study of surface reconstruction and effect on etching behavior; Ref. (Boland, J.J.,1998)Review: electrochemistry of III V semiconductors; Ref. (Gomes, W.P., 1994)Review: wet etching of GaAsH2SO4:H2O2:H2O; review of GaAs etch characteristicsBr2/methanol; review of GaAs etch characteristicsElectrochemical etching of GaAs; review of anodic and cathodic etch characteristics; Ref.(Williams, R., 1990b)3
4A.R. Clawson / Materials Science and Engineering 31 (2001) 1 4382.2. Wet chemical lattice feature delineationEtch pit defect delineation etchantsInPHBr:CH3COOH (1:10); InP defect delineation; etch rate 1:7 mm/min; Ref. (Akita, K., 1979)HBr:HF (10:1); InP defect delineation; etch rate 0:9 mm/min; Ref. (Akita, K., 1979)HBr:HF (1:5) and (1:10); InP dislocation etch pit delineation study with A B etch comparison; Ref.(Kotani, T., 1980)HBr:HF (1:5); InP dislocation etch pit delineation for 5 min at 208C; Ref. (Susa, N., 1980a,c, 1981)HBr:H3PO4 (1:2) {Huber etch}; InP defect delineation; etch rate 0:25 mm/min; gives data on etchrates and etch pit delineation versus etchant composition; Ref. (Akita, K., 1979)HBr:H3PO4 (1:2) {Huber etch}; InP, delineation of pits, ridges, and striations, 1 2 min at 208C; Ref.(Brown, G.T., 1980)HBr:H3PO4 (1:2) {Huber etch}; InP dislocation etch pit delineation; Ref. (Huber, A., 1975)HBr:H3PO4 (1:2) {Huber etch}; InP dislocation etch pit delineation for 150 s; Ref. (Westphalen, R.,1989)HBr:H3PO4 (1:2) {Huber etch}; InP first step etch pit delineation; 1 2 min at 208C givessymmetrical etch pits; followed by H2SO4:H2O2:H2O (1:1:1); InP second step free etch of 30 mm forelongated etch pit delineation for (1 0 0) orientation determination; 5 min at 858C; Ref. (Caridi,E.A., 1984)HBr:H3PO4 (1:2) {Huber etch}; Application: InP and InGaAsP epilayer etch pit defect delineation atroom temperature; Ref. (Nakamura, M., 1993)H3PO4:HBr (2:1) {Huber etch}; Application: InP dislocation etch pit delineation; Ref. (Tamari, N.,1982a)H3PO4:HBr (2:1) (Huber etch); Application: InP defect delineation etch; 2 min at room temperature.CrO3:AgNO3:H2O:HF (1 g:8 mg:2 ml:1 ml) (A B etch); Application: InP defect delineation etch;60 min at 608C; Ref. (Hirano, R., 1993)HBr:H3PO4 (1:2) (Huber etch); Application: InP and InGaAsP defect delineation in 4 mm thickepilayers; Ref. (Nakamura, M., 1993)H3PO4:HBr (2:1) {Huber etch}; Application: InP dislocation etch pit delineation; Ref. (Kimura, T.,1991)HBr:HNO3 (3:1); InP dislocation delineation on (1 1 1) and (1 0 0); Ref. (Chu, S.N.G., 1982)
A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438HBr:HNO3 (3:1); Application: InP (1 1 1) dislocation etch pit delineation; for 7 s; Ref. (Fornari, R.,1989)HBr:HNO3 (3:1); InP dislocation delineation, superior reproducibility to H3PO4:HBr (2:1) {Huberetch}; Ref. (Lourenco, J.A., 1984)HCl:HNO3:HF (5:3:4); InP grain boundary delineation; no effect on first-order twins; Ref.(Hershenson, L., 1980)HNO3:HCl:Br (20:10:0.25); InP and GaP dislocation delineation; 5 s for (1 1 1); 60 s for (1 0 0);Ref. (Clarke, R.C., 1973)CrO3:AgNO3:H2O:HF (1 g:8 mg:2 ml:1 ml) {A B etch}; InP delineation of pits, ridges, andstriations, 30 90 min at 608C; Ref. (Brown, G.T., 1980)A B etch; InP dislocation etch pit delineation; and comparison with HCl:HNO3:H2O (1:3:6) andHCl:HNO3:Br2 (10:20:0.25); Ref. (Huber, A., 1975)A B etch; Layer interface and defect delineation in GaAs, InP, InGaAs, InGaP, GaP; for Ascompounds several seconds at 208C; for P-compounds many minutes at 50 758C; Ref. (Olsen, G.H.,1974)A B etch; Application: InP dislocation delineation; 608C for 20 30 min; Ref. (Takeda, Y., 1980)H2O:AgNO3:CrO3:HF (2 ml:8 mg:1 g:1 ml); A B etch; Application: InP dislocation etch pitdelineation; Ref. (Woodward, J., 1982)AgNO3:HF:HNO3:H2O (40 mg:16 ml:24 ml:32 ml) {R C etch}; Application: InP (1 1 1)B dislocation delineation; etch time a few hours; Ref. (Lee, T.P., 1980)AgNO3:HF:HNO3:H2O (40 mg:16 ml:24 ml:32 ml) {R C etch}: InP dislocation etch pit delineation;Ref. (Takeda, Y., 1978)CrO3:HF:H2O (5:1:x) {Sirtl etch}; InP defect delineation under white or laser light; etch rates for6 x 11; Ref. (Weyher, J.L., 1985)H3PO4:H2O2 (1:1); InP and InGaAs lattice defect delineation with selective photoetching; Ref.(Gottschalch, V., 1982)HCl:HNO3:H2O (1:6:6); Application: InP dislocation etch pit delineation; Ref. (Mullin, J.B., 1970)Anodization: InP; defect delineation; Ref. (Elliott, C.R., 1981)1 M NaOH is electrolyte; n-InP defect delineation electrochemical etch under illuminationH3PO4:HBr (2:1) {Huber etch}; defect delineation comparison; Ref. (Yamamoto, A., 1981)HBr:H2O2:HCl:H2O (20:2:20:20): InP (1 1 1) and (1 0 0) dislocation etch pit delineation; etch pitshape and formation depend on H2O2 and water concentration; shelf time of this etchant is about12 h; Ref. (Huo, D.T.C., 1989a)5
6A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438Defect delineation etchants; Application to InP and InGaAsP: H3PO4:HBr (2:1) {Huber etch} at RTfor 2 min HNO3:H2O:HCl (6:6:1), at 608C for 90 s. HCl:HNO3:Br2 (40:80:1) {RRE etch} at 258Cfor 10 s. H2O:AgNO3:CrO3:HF (10 ml:40 mg:5 g:8 ml) {A B etch} at 758C for 30 min HBr:HF(1:15), at RT for 1 5 min; Ref. (Mahajan, S., 1981)HNO3:H2O2 (1:1); InP {1 1 0} defect delineation etch at 1008C; etch rate 2:5 mm/minK3Fe(CN)6:H2O (15 g:100 ml part 1, and KOH:H2O (15 g:100 ml part 2; part 1:part 2(3:1); InP etch pit defect delineation under illumination for 10 min, etch rate 0:14 mm/min for both(1 1 0) and (1 1 0); Ref. (SrnaÂnek, R., 1993)HF:CH3COOH:H2O2; and H3PO4:HF (1:1); electrolytes for photoelectrochemical defect etch pitdelineation in InP; compared with chemical defects etchant results from: HNO3:HBr (1:3)H3PO4:HBr (1:2) (Huber etch); Ref. (Faur, M., 1993)HBr K2Cr2O7 H2O (BCA etch); InP etch dependence on solution composition; diffusion controlledpolishing etch to kinetically controlled defect etch; Ref. (Weyher, J.L., 1994)GaAsH2O:AgNO3:CrO3:HF (2 ml:8 mg:1 g:1 ml) {A B etch}; GaAs dislocation etch pit delineation. A Betch; Ref. (Abrahams, M.S., 1965)AgNO3:HF:HNO3:H2O (40 mg:16 ml:24 ml:32 ml) {RC etch}; GaAs (1 1 1) dislocation etch pitdelineation. Added AgNO3 reveals etch pits on both (1 1 1)A and (1 1 1)B; Ref. (Richards, J.L.,1960)HCl:H2O2:H2O (1:1:1); GaAs first step surface roughening etch. 10 min; followed by H2SO4:H2O2:H2O (1:8:8); GaAs second step free etch of 50 mm for elongated etch pit delineation for (1 0 0)orientation determination; 3 min at 558C; Ref. (Caridi, E.A., 1984)H3PO4:H2O2 (10:1); GaAs (1 0 0) etch pit delineation and cleaved cross-section layer delineation,3 min under illumination; Ref. (Gottschalch, V., 1979)KOH:NaOH (50 mol%:50 mol%): GaAs defect delineation etch; used at 1708C eutectic meltingtemperature; keeps surfaces smooth compared to molten KOH; shows defects in nominally zerodislocation GaAs; Ref. (Lessoff, H., 1984)KOH, molten (3508C); GaAs (1 0 0) dislocation etch pit delineation; Ref. (Takenaka, T., 1978);(Elliot, A.G., 1987)KOH molten (4508C); Application: GaAs defect etch pit delineation; Ref. (Look, C.C., 1989);(Sewell, J.S., 1989)KOH molten (4008C); GaAs (1 0 0) 10 min for defect etch pit delineation; Ref. (Stirland, D.J., 1986)KOH, molten (4008C); GaAs {1 0 0}; dislocation etch pit delineation; 30 min Ref. (Angilello, R.J.,1975)
A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438KOH molten (3508C); GaAs defect etch pit delineation; relationship of pit density to structuraldefects; Ref. (Tartaglia, J.M., 1991)KOH molten; Application: GaAs (1 0 0) dislocation etch pit delineation. Sirtl etch, modified; GaAs(1 1 1) dislocation etch pit delineation; Ref. (Elliot, A.G., 1987)KOH molten (4008C) for 3 4 s; GaAs epilayer etch pit dislocation delineation; Ref. (Uen, W.Y., 1993)KOH molten; GaAs epilayer etch pit defect delineation; 3 mm etch depth. AgNO3:CrO3:HF:H2O(8 mg:1 g:1 ml:2 ml) {A B etch}; GaAs epilayer etch pit defect delineation; 10 mm etch depth;Ref. (Takagishi, S., 1993)H2SO4:H2O2:H2O (4:1:1); GaAs substrate cleaning for OMVPE growth; 2 min at 508C. KOH molten(3508C); defect delineation; for 5 10 min to reveal etch pits; Ref. (Takagishi, S., 1992)Sirtl etch, modified; GaAs (1 1 1) dislocation etch pit delineation; Ref. (Elliot, A.G., 1987)CrO3:HCl:H2O; GaAs defect delineation study; shows etch characteristics dependence oncomposition; gives high defect sensitivity for low HCl/CrO3 ratios under illumination; Ref. (vande Ven, J., 1986a)CrO3:HF:H2O; GaAs (1 0 0) etch and photoetch defect delineation; Ref. (Weyher, J., 1983a,b)CrO3:HF:H2O (1:2:3); GaAs defect delineation; ultrasonic aided; etch rate at 408C 0.5 mm/min; etchdepth 0.5 2 mm to produce etch pits; Ref. (Chen, N., 1993)HF:CrO3:H2O; diluted Sirtl-like (DSL) photoetching; GaAs; identification of etch features withtransmission electron microscopy; Ref. (Frigeri, C., 1993)HF:CrO3 (1:5) diluted with H2O (1:1) {DSL; diluted Sirtl-like etch with light}; GaAs photoetch, 30 sfor etch pit delineation of dislocations; Ref. (Frigeri, C., 1989)CrO3:HF:H2O; diluted Sirtl-like (DSL) photoetching; Application: GaAs defect delineation; Ref.(Frigeri, C., 1991)HF:HNO3:H2O (1:3:4); GaAs first step etch followed by second step A B etch to reveal growthstriations in LEC material; Ref. (Miyazawa, S., 1982)HNO3:HF:H2O (3:1:4); GaAs delineation of growth striae; 2 min at 208C; Ref. (Plaskett, T.S., 1965)HF:H2O2:H2O (1:1:10); GaAs photoetch dislocation etch pit delineation; Ref. (Nishizawa, J., 1979)A B etch; Layer interface and defect delineation in GaAs, InP, InGaAs, InGaP, GaP; for As-compoundsseveral seconds at 208C; for P-compounds many minutes at 50 758C; Ref. (Olsen, G.H., 1974)A B etch; GaAs (1 0 0) 5 min at room temperature for defect etch pit delineation; Ref. (Stirland,D.J., 1986)7
8A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438A B etch; GaAs dislocation etch pit delineation study; Ref. (Stirland, D.J., 1977)A B etch; GaAs dislocation etch pit delineation. KOH molten at 3008C; GaAs dislocation etch pitdelineation; Ref. (Stirland, D.J., 1978)A B etch; GaAs etch pit defect delineation; 3 min at room temperature; etch rate 3 mm/minNaOH KOH eutectic, molten; GaAs etch pit defect delineation; 30 min at 3508C, etchrate 0:08 mm/min; when used in sequence with A B etch more information is revealed thanwith either etch individually; Ref. (Nordquist, P.E.R., 1993)H2SO4:H2O2:HF (3:2:2); heats spontaneously to 908C. H2SO4:H2O2:HF (1:4:1); H2SO4:H2O2:HF(1:1:2); best shape pits for crystal orientation; for GaAs room temperature etch rate 6 mm/min;Ref. (Kuhn-Kuhnenfeld, F., 1976)H2SO4:H2O2:H2O (10:1:1); GaAs striation pattern delineation in semi-insulating LEC material; 20 30 min at 108C under illumination; Ref. (Fujisaki, Y., 1993)AgNO3:HF:HNO3:H2O (40 mg:16 ml:24 ml:32 ml) {RC etch}; Application: GaAs dislocationpropagation behavior study; Ref. (Yonenaga, I., 1993)NH4OH electrochemical etch; GaAs; dislocation etch pit delineation; comparison with A B etch andmolten KOH etch; Ref. (Wagner, W.R., 1981)NH4OH:H2O electrochemical etch with pH 10:6 13.4; GaAs delineation of striations, dislocationsand twins; Ref. (Green, L.L., 1977)CrO3:HF:H2O (DSL, diluted Sirtl-like with light photoetch); defect delineation in GaAs; comparisonto EBIC images; Ref. (Frigeri, C., 1990)H2SO4:H2O2:H2O (20:1:1); GaAs striation delineation etch. H2SO4:H2O2:H2O (15:1:1); GaAsstriation delineation etch. H2SO4:H2O2:H2O (8:1:1); GaAs striation delineation etch. AB etch; GaAsstriation delineation etch. AB:H2O (1:5); GaAs striation delineation etch. Diluted Sirtl etch; GaAsstriation delineation etch; Ref. (Pandelisev, K.A., 1990)Bi(NO3)3:H2O2:HCl (0.38 g (Bi(NO3)25H2O) in 15 ml H2O2 mixed with conc. HCl in the ratio 3:1);subsurface defect delineation on polished GaAs; Ref. (Sankaranarayanan, K., 1997)CrO3:HF:H2O (DS, diluted Sirtl-like etch and DSL diluted Sirtl-like with light photoetch); defectdelineation in GaAs; comparison to KOH (molten) defect delineation; Ref. (Weyher, J.L., 1986)DSL (dilute Syrtl like) etch to reveal As precipitates for TEM study; Ref. (Weyher, J.L., 1998)InGaAs(P)H2O:AgNO3:CrO3:HF (10 ml:40 mg:5 g:8 ml) {A B etch}; InGaAsP LPE layer defect delineation;25 min at 658C; Ref. (Shirafuji, J., 1981)A B etch; Application: InGaAs dislocation etch pit delineation; Ref. (Ahmad, K., 1979)
A.R. Clawson / Materials Science and Engineering 31 (2001) 1 438A B etch; Application: dislocation delineat
Review: GaAs etching overview; wet and dry etching; Ref. (Ashby, C.I.H., 1990a) Review: InP wet chemical etching; with (1) defect or damage revealing etchant table, (2) polishing etchant table, and (3) pattern etchant table; Ref. (Adachi, S., 1990b) Review: wet and dry chemical etching of GaAs; classifies wet etchants as non-electrolyte (those with
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Abattage des roches b. Foration c. Tir d. Chargement et transport CHAPITRE III CALCUL DE LA STABILITE DES TALUS DE LA CARRIERE DE AIN EL KEBIRA III .1. INTRODUCTION III .2. DETERMINATION DES PROPRIETES MECANIQUES DES ROCHES III.2.1. Résistance a la compression III.2.2. Résistance a la traction III.2.3. Cohésion et angle de frottement interne d’un échantillon III.2.4. Fissuration des .
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Index of Resolutions from 1998 Section III.4 - Eames Commission Section III.5 - The Authority of Holy Scriptures Section III.6 - Instruments of the Anglican Communion Section III.7 - The Lambeth Conference Section III.8 - The Virginia Report Section III.9 - Inter-regional groupings Section III.10 - Ma
