Surface characterization - ACS Publications - American Chemical

AMI.

-.Mao.

(473) Mne. R. W.: and Omas. (474) Palion. J. G.: A W , M. C.; lo"-.)n" 1,oe.x .qCL"" I Is"C,.

(475) MaO. (1982).

S.J. T.; and Omas. -.

chsm. 1986, 57, 130R-151R

3. 23-30 (1983). S. J. 1..J . I m M o l . Mshodb. 55.

W m . Am.

7i3. 3 6 5 4 7 4

(478) KoUmrb. N. M.;and Omas. m.m.. 30. 1539-1545 (1984). ( 4 7 z ) a e 2 m , R.: Bradslrav. R. A,. Ann. Rev. Pkehsm.. 55, 259-282 (478) Amrm. A,: and Omas. Roc. M U . A&. (1984).

sd..S A . 81,2176-2180

Surface Characterization R Allen Bowling,' Thomas J. Shaffner, and Graydon 9. Larrabea Materials Science Laboratory. Texas Instruments. Incorpomted, P.O.Box 225936,MS 147, Dallas, Texas 75265

Thia review will have a different format from earlier revim

(1194-1197). Thin change is an effort to make the review more

readable and more readily understood b the reader. Aa a result, more use will be made of tables. 6ertain sections d o nnt fit a tnhle format and will be the m e 88 in earlier reviewa The authors encourage constructive commente and criticism of the new format. T h e abbreviations used for the various characterization techniques are shown in Table 1. As before. this review attempts to cover the technical literature appearing during the last 2 years sinre the last review. Reference begin with October 198" and end with November 1984.

R. Alan Bommg lohsd T e r n lnamnmma. I-ated. h ssptembsr 1980 as a pro. w m o l h a umlconducm pocssskg area. In J m m y 1982 he bb cams m a n k Of thetschlcal Nff h the Materials Characleriratlon branch 01 the Materials Science Laboratory and was. unul Jub 1984. reaponeibie f alechnka S u p V C sbn of scanning A and A-lXPS bboralaiss. He k curenay wuking h me Mataiak tor VLSl bench 01 me Matsrlak Science L a b o r a h y on me development of new pmcessss fa M u e devlce fabrication. Before Jdnkg TI. Bowling hM an Alexanja y o n Humbddt pasldoaaai research posraOn SI lhe lnstnute of lnagsnic Chemistry. Unkersny of FrankM. Frankfurt. Wosl *many. Ha r-ked lhe w e e B.S.in chenxSby from the Unkersw of Alabama in 1975 and was awarded a Ph.0. in chemistry by lhe Unksrrny of Tennes- h 1979. Bowllng Io a memba of me Eie)CbochBn*CBI Society. me Amedcan Vacuum Society. and lhe North Texas Mat~rhisChara~lerlza. tbn Society. He hap published p a w s In a number of technical @Is and has a b made pesentetionr on materiak ChamCterlLBtb" memods at SBvMBI r e g h l and n a t h l technical meetings.

Tabla I. Abbreviations

AES APS A6 ELL EELS EMP EPR ESD ESR EXAFS FEM FIM IMMA ISS LEED MS N MR

moM. J. oh*hr !d mm@a o( the Mat&* charactukation Branch of me

RBS

h t & k SClence Laboratay Of Texas In(Ib"me"B. 1ncaporated. He pfned the company h 1977 as head 01 the Svtacs Science and Eleclron Spsnoscopy a& w. and wan en@@ h mmputer au1MB. Um of AvpalXPS InsrmmentadDn and applC catbns Of sufacbsonsnlYe techniques to p o b h SOMng. He subsequentty assumed r e s w W as manager 01 electrm beam and X-ray imagaphy efforts in me VLSl labaatory where devebpmems in VHSIC reucie and SK: X-ray mask techwere knplemented. 10 tMs. he w a k e d at Du Pom apphling scanning 6ech-m mlcrmcopy. X-ray analysis. end lnhared im aging techniques lo p4ymedc materials and processes. Shatma earned a B.S. In phyrks from N& CBrdlna Stale Unkersity in Raleigh. NC. and a R.D. in physics horn Vanderbin Unkerow. He has publlshsd In physks. h s m n i a t b n . and Chemical ]amals. end mtrfbuted chapters in books. He Is a memba 01 the AAAS. Amer!an ClyNllOgaphk AssociaUm. M~CTP bsam Analysb Society. American Vaeum Society. SPIE. and m w -09 a8 Chahnan 01 lhe North Texas Sectbn 01 me Electrochemical Society.

RHEED SAM SEM SIMS TD TEM UHV UPS XPS XRD XRF

m

130 R

0003-2700/85/0357-13OR$O8.50/0

Auger electron speWoseopy appearance potential spectroscopy change in work function ellipometry electron energy loss spectroscopy electron microprobe analysis electron paramagnetic resonance electron stimulated desorption electron spin resonance extended X-ray absorption fine StNCtUre field emieaion microscopy field ion microscopy ion microprobe masa analysis ion scattering spectroscopy low-enerw electron diffraction mass spectroscopy nuclear magnetic resonance Rutherford backscattering reflection high-energy electron diffraction scanning Auger microscopy scanning electron microscopy secondary ion mass spectrosropy thermal desorption transmission electron microscopy ultrahigh vacuum UV photoelectron spectrosropy X-ray photoelectron spectroscopy (ESCA) X-ray diffraction X-ray fluorescence

METALS Alkali Metals. The adsorption of oxygen and water on dean lithium surfaces w88 stuhed with XPS. and quantitative reaction raten were determined (455).The reaction producta 0

1985 Amsrican chermcal S O C W

SURFACE CHARACTERIZATION

Table 11. Surface Characterization Applications to Copper and Its Alloys element copper

Cu alloys Cu-Ni

surface reconstruction

elemental gases

3, 264, 320, 361, 514, 646, 647, 734, 770, 774, 988, 1047, 1054, 513

HZ 394, 718, 840, 785 He 692, 840 0 2 484, 1052, 60, 888, 9, 530,733 C1566, 1143, 1144 Ar/Xe 250

02 90,658

chemisorption elemental solids

K 23 S 648 Fe 84 Co 736 Ni 1065 Pd 237 Sm 308 Pb 171,800, 21 Sn 21 Te 512

molecular HZO 48-50, 395, 396, 683,853 CO 462,463, 495, 707, 1119, 1157, 1127, 975, 1127, 975 H2S 852 HCN 972 M0,0?4 830 organics 434, 727, 252, 1020

UV emission 688 core energy 1130 diffraction 1133

CO 719

surface composition 521. 1050 segregation 151 segregation 338 segregation 437 segregation 147 surface composition 980 segregation 438 oxidation 485 surface composition 1094, 1093

Cu-A1 Cu-Si Cu-Mn

02 437

CU-AU

0 2

389

0 2

686

Cu-Sn Cu-Zn Cu-Pt Cu-Rh Cu-Ag

formed on clean lithium surfaces exposed to acetylene gas were examined by using UPS and AES (359, 360). The LEED pattern from sodium evaporated on Cu(100) a t 77 K was recorded and compared to theoretical patterns (645). Photoemission studies of the oxidation of cesium a t -140 K identified four different states of oxygen (1005). Angle-resolved UPS studies of xenon physisorbed on cesium surfaces were reported (902). Light Metals. The intrinsic surface state on Be(0001) was recorded with angle-resolved photoemission spectra excited by 24-30 eV synchrotron radiation (534). Both LEED and AES were used to characterize the initial stages of oxidation of the Be(0001) surface (196). The oxidation of polycrystalline boron was studied with EELS and AES (895) and both elemental and oxidized boron were present on the surface. Raman scattering was employed to show that a continuous transition from the crystalline to the amorphous takes place for phosphorus (808). Clean (0001) and (1100) faces of magnesium were investigated with EELS (368)to study the low energy inelastic scattering properties. Scattering of CkeV Ar+ from Mg(0001) was interpreted in terms of “zigzag” collision sequences on the surface (535). The interaction of gaseous hydrogen with clean and oxidized magnesium surfaces was studied with time-of-flight analysis of recoiled surface atoms produced by pulsed Ar+ irradiation (735,928). It was found that oxidized magnesium reacts with hydrogen to yield a product with a surface stoichiometry of approximately one hydro en to one MgO pair. The oscillatory relaxation of Al(1107 surfaces was examined with LEED (14,776,788).The nature of the excited states of rare-gas atoms adsorbed on Al(111) was determined with EELS (250). The interaction of CO with Al(111) was studied with AES, LEED, and EELS (553). LEED was used on the Al(111) surface to study the structure during the initial stages of interaction with oxygen

other

co 944,945, 946, 1013 ethene 1095

photoemission 717

surface composition 1015 surface composition 1015

(689). Reflection EELS was carried out on aluminum samples with excitation energies in the 30-1000 eV primary electron range (189). A medium-energy electron diffraction (MEED) technique was applied to Al(001) a t 77 K to confirm that no relaxation occurs a t that surface (698). The ion energy distribution of H+ ions was determined with electron desorption spectroscopy (EDS) of water adsorbed at room temperature on Al(100) and interpreted in terms of an Auger decay process with OH groups a t the surface (269). An atom-probe study, which investigated hydrogen physisorption on aluminum, detected metal hydrides on the aluminum surface (785). The electronic structure of oxygen on Al(111) surfaces was reviewed (74, 75). The initial stages of chemisorption of oxygen on aluminum favors the view that oxygen atoms are cited on the top plane of Al(111) (882). The effects of electron irradiation on oxygen-exposed aluminum were investigated with AES and a “Coulomb explosion” decomposition and desorption mechanism proposed (5). Surface extended energy loss fine structures were detected above the K-ed e of oxygen adsorbed on an aluminum sample (239). The afsorption of water on Al(111) was studied with ESD, LEED, TD, and AES (769). The role of water on the aluminum surface in corrosion was investigated with XPS, UPS, LEED, and EELS (1029). The growth of oxide on aluminum films in the presence of keV electrons and carbon dioxide was studied with AES,X P S , ISS, and SIMS (862,307).The oxidation of aluminum-magnesium alloys was measured (624, 631). AES was used to measure the low temperature surface segregation of silicon in aluminum-silicon alloys (2). A perfect monolayer of Sm on Al(100) was shown to be composed wholly of trivalent ions using LEED and XPS (309). Mixed-valent Yb on Al(110) was established with AES, EELS, and XPS (810). The bonding of a simulated epoxy resin to aluminum surfaces was studied with XPS (125). Applications of AES and XPS to the surface ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985

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Table 111. Applications to Iron, Cobalt, and Nickel and Their Alloys

element iron

surface reconstruction 263,297,680,969, 970


elemental gases Hz 786, 793, 128

Se 757

O2 11,235,617,557, 380 Fe 627

Nz492,732, 718,778 Br 751 Fe alloys Fe-Cr

0 2

Fe-B-Si Fe-Si Fe-Si-Sn Fe-Co Fe-Gd Fe-Ni-Co Fe-Cr Fe-Ti steels

510

Te 758 C 867

NH, 303, 304

02 565

oxidation 815 segregation 275

inconel

so2 347

HZS-NZ 348 CO 1033 CO 1033

H2 1033 1139

O2 121, 163, 526, 1124

C and S 674

132 R

bonding 193 71,93, 200, 206,319, Ne 130 S 17, 78, 117, 118, 880,378 CO 187, 216, 331,879, 495, 373, 472, 537, 706, 362, 406, 500, 517, 615, 921, 921, 97,638, 1058, 1064, 1067, 1125, 504 749, 1107, 1054 He 891 H2 916,987, 501, 755, C 881,899,471 780,809,838 Nz276, 295,296,97, 404, Te 512 407, 504, 717,405 C1 667 CO and Hz 166, 214, K/Hz 1011 738, 832, 835, 778, 665,1012,573,574, 603 c u 744 c u 744 12 519,976 CO/K 664 0 2 366,422,423,486, 504, 699, 1030, 30, 1044, 1116, 61, 97, 1154, 342,889, 274 CO/Ni(CO), 375,620 Hz/OZ 1113, 1114 COz and Oz 85, 914, 1115 H20 92, 161,834, 1076 NH, 133, 327,403,485, 507 NO 132 organics 96, 267, 268, 67, 418, 47

Ni-Fe-P NiFeCrPb

segregation 4 surface comp. 961, 962

CzHz 8 CO 343, 827, 73, 393, 414

Co alloys Sm-Co

Ni alloys Ni-A1 Ni-Cr Ni-Fe

photoemission 316, 909

polishing 24 corrosion 481 surface comp. 1040 segregation 288 segregation 1190 sputter 108 crystal 626

o21112

Hz 1033

nickel

other

CO 127, 778, 511, 602, work function 446 933, 1132, 128 COZ 290 passivation 655 HzO 444,445 organic 703, 934, 1131, 1147

S 760

323

cobalt

molecular

0 2 244 He 383

0 2

P 533 S 681, 682 S and Oz 604

536

ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985

polish 229

work function 1056 crystal 1110 energy loss 529 magnetic 315

photoemission 257 plasmon 819

bonding 238 surface tension 63

oxidation 1180 segregation 584 CO and Oz 197 polishing 25


Table IV. Applications to the Refractory Metals and Their Alloys element



molecular

02 335, 1137

vanadium molybdenum

elemental gases

321

0 2 79,346,

C 818

818,310 NZ 45 HZ 310

CS/Oz 893, 979 S 365,911, 912

CO 310 NH3/N2 292 organics 729

niobium Nb-Ge

02 399 02 491

rhenium

N2/02 555

CO 281 H2O 522,523

C12/12 998

CZHz 654

tantalum Ta-W-Hf

1055

tungsten

261, 262,321, 325,449, 520, 554,822,990, 1123, 1140, 1156,398, 1122

tungsten bronze

02 230

HZ 468, 1099, 261,262,468, 1099,951 H+/H- 650 Hz/OZ 469 He 777 Nz 31,398, 405,1077,951 02 59,1122 Kr 1187 Xe/Kr 812, 813 Cl/Br 122

S 496,869 Si 428,1141 K 80,81 Ba 318 Ba/O 336,607, 608,687

CO 470,495, 811, 1078

NO 728 NHB 294 C2HZ 337

Ag 981 Ag/Au 582 Bi 518 Fe 1120 Se 868

756

characterization of aluminum and its compounds were described (1041).Aluminum deposited on Sic a t room temperature was shown to form quasi-metallic islands randomly distributed over the surface (99). The stoichiometry and thickness of the initial oxide formed on clean titanium surfaces were determined by quantitative AES,UPS, ESD, EELS, and microgravimetry (102,103, 152). Oxygen adsorption and coadsorption of lead and oxygen on polycrystalline titanium was studied with AES. Hydrogen and oxygen adsorption and sulfur se regation on a clean titanium surface was measured with AE! and EELS (837).The kinetics of nitride formation on titanium targets during reactive sputtering was measured with AES (1017). The basal plane of titanium was studied with low energy electron current image diffraction (58). Copper. The applications of surface characterization to copper and its alloys are shown in Table 11. Chromium. The structural properties of clean Cr(100) surfaces were examined by LEIED, XPS, and A 4 (335).The photoelectron spectra of chromium metal was measured in the excitation range from 30 to 80 mV a t room temperature (1007).Measurements were made of the electron and positron work functions of submonolayer contaminated single crystal surfaces of Cr(100) in ultrahigh vacuum (1153).The reaction of bromine with Cr(100) was studied with AES, LEED, A$, and T D (334,886).The chemisorption of oxy en on Cr(100) was studied with LEED and XPS (76,367).8pin-polarized photoemission was employed to study oxygen-induced ma netism in a Cr(l00) surface (856).X P S studies of hexafhoric!e complexes of chromium(II1) were performed (332).The adhesion of polyimide to chromium surfaces was investigated with XPS and TEM (194).Surface segregation of chromium in an iron-chromium alloy was characterized with XPS (275). The valence band of chromium-aluminum solid solutions was determined with AES (622). Iron, Cobalt, and Nickel. The applications of surface characterization to iron, cobalt, and nickel and their alloys are shown in Table 111. Refractory Metals, The applications of surface characterization to the refractory metals and their alloys are shown in Table IV. Polarization (580),backscattering (712),and electrochemistry (906) of the tungsten surface have also been studied.

Precious Metals. The surface characterization studies of precious metals during the past 2 years are summarized in Table V. The growths of epitaxial thin films of palladium have been studied (237,1091).The surface compositions of the alloys Pd-Ge (149),Ag-Sn (428), and Ag-Mn (521)have also been studied. Other Metals. Temperature-programmed desorption of hydrogen on Zn(OOO1) surfaces (173)showed adsorption in its atomic state. The oxidation of zinc in air was studied with XPS and AES (420).The adsorbed oxygen was found to be in two different valence states. RHEED, LEED, and AES were used to understand the interaction of sulfur dioxide with the Zn(0001) surface (353). Surface oxidation of niobium under a UV laser was studied with XPS (684) and revealed a range of niobium oxidation states. The Auger spectrum of technetium was determined (184,619). The adsorption of oxygen, nitrogen, carbon monoxide, and nitrous oxide on polycrystalline zirconium was investigated with AES and XPS over a wide temperature range (457). Electron and ion emissions from chlorine and bromine chemisorption on yttrium, titanium, zirconium, and hafnium surfaces were characterized (210,21 1). The chemisorption of hydrogen, oxy en, and water on lathanum was studied with XPS and U P 8 (598).The chemisorption of chlorine and sodium and their coadsortion on polycrystalline foils of yttrium and scandium were investigated with AES,TD, and A4 (236).The oxidation of liquid and solid tin from 298 to 513 K was investigated with EELS and AES (110,982).LEED was used to establish the surface structure of a-Sn(100) and its interaction with atomic hydrogen (1158,1159).The oxidation of barium surfaces and their behavior was extensively investigated (370,412,413,949). The reaction products and subsequent thermal decomposition of barium films exposed to carbon monoxide, carbon dioxide, water, and oxygen were determined with AES and T D (050). The generation and pumping of h drocarbon gases by a barium getter layer were investigated i y characterizing a barium film in UHV using XPS before, during, and after ex osure to methane, ethylene, acetylene, and ethane (1108).ZPS and EELS were used to study the oxidation of lead (1045). Ordered steps on B(--oOOl) surfaces after pulsed excimer laser annealing were characterized with LEED (300).The interaction of oxygen with clean ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985

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Table V. Surface Characterization Studies of Precious Metals element gold


502, 596, 890, 114, 115, 1164, 742, 1183,301, 954

elemental gases

858, 859, 159 Ar 250 Xe 250 0 2

K 311 Pb 356 Bi 356

614, 107, 577

02 591, 847

osmium

Nz 442

palladium

Hz 558, 753, 870, 795, 796, 797, 798, 1135, 165, 94 02 1003, 1134, 796, 1002, 795, 1135, 797 Nz 442 c1943

C 552

HzSOd 849 A1203144 sulfides 10

502, 605,625 775,73

Hz 363, 556, 905, 72, 218, 915, 128 0 2 221,

223, 918, 227, 228, 397, 374, 630, 714, 861, 704, 705, 789, 791, 792, 848, 850, 1014, 41, 1021,985, 222, 256, 821,820 Nz 509 442

organics 1032

CO 1106

Br 651 Au 597, 1136 Si 402, 98 Ag 160

CO 364 558, 737, 870, 767, 1003, 141, 143, 495, 1165, 1086, 885 Hz 796, 1002 NO 923, 242 organics

358, 550, 581, 652, 551, 82, 1704, 938, 47, 506

Xe 1121

platinum

molecular

Au 1136

Au-Pd iridium


s 578,

940, 113, 772, 1, 30 K 560, 128, 41, 561,861 19 Cs 41 Zr 54, 56 Ag 1148, 994,992

Iz 971, 991,994 c u 947, 1174, 991 Si 1092, 820,821

HzO 219, 221, 222, 538, 223, 803, 218, 618 co 374, 87, 88, 376, 377, 430, 431, 560, 828, 790, 791, 865, 866, 19, 38, 1191, 51, 1066, 57, 1048,986, 104, 209, 932, 495, 128,821 COZ 700

NO 227, 429, 464, 559, 561, 828, 51, 930 NO, 227, 714 so2 579, 27 organics

Pt-Ni

134R


220, 226, 344, 345, 363, 459, 509, 538, 556, 836, 905, 19, 33, 34, 35, 36, 1019, 39, 1096, 939, 1018, 941, 695, 37, 1020 H2P04 416 CzHs 695 CzH4 695


Table V (Continued) element rhenium

rhodium

ruthenium

surface reconstruction 585

1089, 1090

724

elemental gases O2 1042

chemisorption elemental solids K 585

CO 1043

Fe 585 C 471 Ag 13

organics 12,471

Hz 225, 799, 215 02 328, 846, 897, 935 Nz 799, 442

K 224 A1 935

H20 224, 352, 453, 833 CO 1166, 1089,904, 1191, 898, 1090,833, 215, 245, 246 NO 452, 453, 799, 897,898 organics 572, 575, 643, 562, 936, 1096, 973, 974

Hz 64 02 270, 432, 639, 590,989 Nz 715, 18, 1077

Na 271 272, 768 C1410 C 825 K 253 Cu 142,

HzO 270, 272 CN 409 CO 724, 715, 768, 825, 44, 1167, 977 NO 293, 432, 989, 208 organics 322, 293, 456, 478, 669, 40, 91

1111

silver

433, 656, 666, 609, 610, 675, 592, 764, 6, 1182, 260,438, 1183, 379

molecular

02 299,

324, 390, 564, 589, 157, 845, 844, 877, 592, 817, 873, 20, 29, 41, 43, 530, 65, 66, 924, 89, 249, 530 Hz 249 Xe 694, 746, 250 Ar 746, 250 Kr 694, 746 C1 131, 67, 513,530

Bi(OOO1) surfaces was studied between 118 and 296 K using LEED, AES, and A$ (1046).The interaction of chlorine with Bi(OOO1) was measured with LEED, AES, EELS, TD, and A$ (158). The adsorption of methyl iodide on uranium and uranium oxide was characterized with XPS and AES (26). Surface segregation in liquid Ga-Sn alloys was measured with AES (425,426).AES was also used to study surface oxidation of molten solder (243). The characteristics of magnetronsputtered high atomic number amorphous metal alloys were performed with AES (111).

Li 433 K 433 41 c s 433, 41 12 675, 55 Pb 896

Cu 260 Pd 967 Ag 131,67

H20 564, 668, 694, 863, 65 CO 157, 43, 495, 1127 COZ 157, 43 KOH 845 NO 86, 242 organics 390, 324, 593, 670, 693, 694, 817, 873, 864, 112, 43, 1129, 1004, 924, 249, 185, 199

SEMICONDUCTORS Surface characterization studies of semiconductor surfaces have flourished during the past 2 years. In addition to growth in the silicon area, there have also been large increases in the number of studies of group 13-15 and other compound semiconductors. Silicon. The references to studies of surface reconstructions of Si and chemisorption on Si are summarized in Table VI. The category on adsorption of elemental solids on Si ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985

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Table VI. Surface Characterization of Silicon chemisorption elemental solids


elemental gases

Si(100)-2 X 1 168,460, 1068 Si(OO1)-2X1 1172 Si(lll)-2Xl 314, 424,448, 476, 497,649, 702, 317, 188 Si(lll)-lXl 251,448,465, 570, 710, 711, 1170 Si(ll1) 22, 742 Si(100) 515, 516

Hz 205,547, 567, 251, 167, 571, 317, 690, 691, 919, 920,922, 1001, 662 He 357 02 461,920,922,372,662,917, 1186 NZ 927, 926 Xe 207 Kr 207 c1202 I202

molecular

Te 202 Li 392 Na 392 K 392, 1060 Cs 392 Ga 123 In 123 A1 137 Sb 721 Yb 576 Sn 487, 1075 Au 137, 251, 254, 474,475, 499, 1162 Ge 181, 183,385, 386,489, 955,956,957 Ni 176, 177, 204, 371, 773, 781, 784, 782, 1073, 1173, 402 Ag 465, 466,467,473, 587, 632, 996, 421, 1097, 1098, 1178 Pd 204, 247, 251, 807,816, 402, 1069, 1163,1070 Ti 498, 153 Mo 771 W 783, 784 c u 900 Pt 402 Ta 180, 823 Cr 823 Co 860

H20 116, 201, 802,920, 922,999

DzO 999 NO 779 HF 569 NO2 595 A1203 144 ethene 567 methanol 291 silane 722, 1181 phosphine 722, 1181

Table VII. Miscellaneous Silicon Surface Characterization description of studies

ref no.

study of clean silicon surfaces study of cleaning procedures for Si(100) surface surface defect analyses surface analysis of sputter-etched silicon solid phase epitaxy of silicon thermal oxidation and nitridation of silicon oxide growth rat on Si(100) in air anodic oxidation of Si in methanol and glycol electron-activated oxidation and nitridation of Si MBE deposition of silicon oxides on silicon analysis of iron oxide coated silicon photoanodes photodesorption of COz from oxygen-saturated Si(100)

62, 1186 421 443 804, 964, 842 588, 541 255,676 713 672 568 677 787 1087

includes references which pertain to the formation of metal silicides. These silicide references will also be included later in the section on other metal compounds. Several other miscellaneous characterization studies of silicon surfaces were also carried out during the last 2 years. Each of these is briefly described in Table VII. Group 13-15 Semiconductors. The references to studies of surface structure and reconstruction, and to chemisorption of species on group 13-15 compound semiconductor surfaces are summarized in Table VIII. The surface characterization studies of group 13-15 compound semiconductors which do not relate to structural or adsorption studies are summarized by brief descriptions and reference numbers in Table IX. Other Semiconductors. Chemisorption and surface structure reconstruction study references for the past 2 years for semiconductors other than silicon and group 13-15 compound semiconductors are summarized in Table X. The miscellaneous nonstructural and nonchemisorption studies 136R

ANALYTICAL CHEMISTRY, VOL. 57,

NO. 5,

APRIL 1985

of semiconductors other than silicon and group 13-15 compounds are summarized in Table XI.

OTHER MATERIALS Metal Oxides. The structural investigations and chemi-

sorption studies of metal oxide surfaces during the past 2 years are summarized in Table XII. A general review of chemisorption on transition-metal oxides can be found in ref 441. Table XI11 is a compilation of the surface compositional studies of metal oxides which were performed during the past 2 years. Other Metal Compounds. The surface studies of other metal compounds durin the past 2 years are summarized in Tables XIV-XVII. Ta%le XIV is a compilation of surface structural investigations and chemisorption studies. Table XV is a summary of surface composition studies. Table XVI is a list of surface oxidation studies, and Table XVII is a review


Table VIII. Group 13-16 Compound Semiconductor Surface Studies surface reconstruction

elemental gases

GaAs 503 GaAs(100) 742,913 GaAs(001) 763, 1026, 1027, 1085, 1088 GaAs(ll0) 169, 282, 287, 387, 388,480, 524 GaAs(ll1) 1063 GaAs(2ll) 479 GaP(110) 284, 524 GaSb(ll0) 285, 283 GaSb(ll0) 285, 283 InP(100) 742 InAs(ll0) 286 GaInAs 903


on GaAs(100): on GaAs: Hz 138, 139 Ge 1000 Mo 1008 on GaAs(ll0): Si 540 Hz 70 O2 69, 70, 100, 339, 340, 611, 660, 883, 884 on GaAs(100): on GaAs(ll1): Ge 750 Hz 138, 139 Pd 801 on GaAs(001): Cs 894 02 329 Ag 280 on InP: Fe 531, 532 on GaAs(ll0): 02 1117 on InSe: A1 1188 0 2 739 Sb 965 Cu 824, 124 Ag 663, 824 Au 387,824, 843 Pd 387, 801 Ge 182 on GaAs(001): A1 15, 16,612, 1026 Au 761 Ge 762 on GaAs(ll1): Cs 894 on GaP(110): A1 126, 525 on InP(110): A1 525, 548, 1188 Ga 1151 Sn 1151 Sb 1151 Pd 549 Au 42 Ni 483 Cu 483

molecular on GaAs(ll0): HzO 100, 190, 743 formic acid 701 CO 100,340 NO 100 ZnSe 287 on InP(110): HzO 745 on InP(100): BaF2 851 on InP(111): BaF, 851 on InP: Si02105 on GaAs: Si02586

Table IX. Miscellaneous Surface Characterization of 111-VSemiconductors description of studies

ref no.

EELS of sputter-annealed GaAs, InP, and GaP metal-organically grown anodic oxides on GaAs AES of MBE grown AlGaAs/GaAs superlattice EELS of Te-doped GaAs(100) after Ht ion bombardment XPS of thermally oxidized InP laser-induced desorption of P from GaP AES of InP after oxidation and Art ion bombardment XPS of GaAs(100)thermally cleaned in UHV composition of epitaxial ZnSe on GaAs(ll0) Schottky barrier heights on GaAs(100)and AlAs(100) composition of H2S04/H202cleaned GaAs(100) study of InSb(100) thermally cleaned in UHV native oxide formation on InP characterization of CVD BN on InP study of photochemically passivated GaAs surface study of InP(110) after Art ion bombardment composition of annealed anodic oxides on InP composition of GaAs(100) after wet chemical etching analysis of plasma-grown oxyfluorides on GaAs XPS of AlGaAs surface composition study of growth of InGaAs on GaAs(100) photoluminescence transients on GaAs(ll0) thermal restructuring of oxides on GaAs and AlGaAs MBE grown InAs/GaSb and Ge/GaAs superlattices observation of As segregation on GaAs(ll0) GaSe and InSe work function after Art ion bombardment surface composition of air-oxidized GaSb

279 369 302 278 765 759 942 1031, 1102 1072 1126 1101 1102 1117 1168 1155 831 312 482 493 494 640 129 150 174 68 1039 740

ANALYTICAL CHEMISTRY, VOL. 57,

NO. 5,

APRIL 1985

137R


Table X. Surface Structure and Chemisorption Studies of Other Semiconductors surface reconstruction

elemental gases

Ge(100)-2~1 731 Ge(001)-2~1 766 Ge(ll1) 1177 Ge(ll1) 1177 Ge(lll)-2x8 878, 1176 Ge(ll1)-2~1 878, 892 GeSi(ll1) GeTe 1035, 1037 GeSe 1035, 1036 ZnS(110) 284 ZnSe(ll0) 287 ZnTe(ll0) 283 CdS 995 CdTe(ll0) 841 CdTe(ll1)A 841 CuInSez 508, 594

on Ge(100): Hz 1022 02 1023, 1024 on Ge(ll1): Hz 1022 on HgCdTe: 0, 959 on CuInSez: 0 2 508


molecular

on Ge: Si 540 on Ge(001): Ag 644 on Ge(100): Ag 730 on Ge(ll1): Ag 632, 1009 Pb 720,488,634, 635 Sn 910, 447,487 A1 539 Au 633 on CdS: Si 540 on PdTe(100): Ge 166 A1 166 In 166 on HgCdTe: Au 231 A1 232 Ge 232 on ZnTe: Au 953

on Ge(100):

BaP, 851 on Ge(ll1): BaF, 851 on Ge(001): GaAs 762 on Ge(ll0): GaAs 1192

Table XI. Surface Studies of Other Semiconductors description of studies

ref no.

composition of CuMoSe grown by the Bridgman method composition of sputter-depositedBizTeaand PbTe composition of anodic films on HgCdTe composition of air-exposed CdTe(ll0) evaluation of SnSe thin polycrystalline films composition of native oxides on HgCdTe anodic films on HgCdTe after Ar+ ion bombardment MBE growth of HgCdTe cathodoluminescence characterization of ZnSe composition of cleaved and sputtered CuInSe, oxidation of CuInSe, XPS study of amorphous silicon-germanium alloys spectroscopic investigation of amorphous InTe composition of air-annealed CdS films study of thermal stability of anodic oxides on HgCdTe photoemission study of InSb(001) and Sn(001) composition of cleaved, oxidized, and heat-treated CdTe composition of photochemically grown oxides on HgCdTe composition of PbTe(100) after etching and Ar+ ion cleaning MBE growth of CdTe films on hydroplaned CdTe Raman study of crystallization of amorphous Ge composition of mixed CdS-CdSe films

of the other miscellaneous surface studies which do not fit any of these other categories. Carbon-Based Materials. Surface characterization studies of carbon-based materials are detailed in Table XVIII. Glasses a n d Ceramics. XPS continues as a major characterization technique for the study of glasses because of its unique abiility to determine chemical bonding information without the problems associated with static charge buildup on these high resistivity materials. Studies have focused on the simple determination of constituents, such as K in lead silicate (960) and silicon nitride in soda-lime glasses (140), as well as the bulk dissolution, leaching, and surface enhancement and decomposition of vitreous silica (621), Zn (641),and Cu-Ti (436) containing glasses. An XPS study of Fe and Ni metallic glasses has compared the oxidation behavior with their nonmetallic counterparts (937). The effects of a glass substrate on the deposition of thin films of precious metals have been studied. Work function changes in Pt films evaporated on smooth quartz and Pyrex were attributed to the formation 138R


1038 952 931 1142

95 26 197 195, 313 191 696 542 661 606 583 527 454 427, 887 233 806 754 1175 52

of Si-0 groups at the surface (1092), and the surface morphology of deposited Au and A films was shown to depend on temperature of the lass su%strate (1183). The decomposition of glasses cause by electron and ion beam irradiation has been studied. XPS was used to show reduction in Na and 0 signals, the latter being attributed to desorption of both bridgin and nonbridging oxygen (876). The same technique found tiat 5-keV Ar+ bombardment of lead oxide coneining glass resulted in preferential sputtering of lead over silicon and a reduction of lead to its metallic state (198). EXAFS was used in a synchrotron study of the electron density environment around the silver ion in a silver borate glass (101). Catalysts. A variety of analytical techniques have been used in catalytic studies, including both bulk and surface sensitive methods. The precious metals Pt and Ru can be found in many studies concerned with catalytic systems, and several publications that specifically focus on the catalytic functions are mentioned here. However, the many articles included in the prior Table V dedicated to previous metals

d


Table XII. Chemisorption and Structural Investigations of Metal Oxides structural investigations

elemental gases

ZnO 503,505 MgO(100) 1138 MgO(001) 146,1081, 948 NiO(001) 330 NiO(ll1) 330 Sn02 241 Tiz03708 Mo0,(010) 162, 326 Fe203601 UOZ 1051, 1053

on TiOz H2 382 O2 382 on Ti203: O2 600 on V203: O2 600 on FepO$ O2 600 on Zn 0: Xe 451 0 2 186 on Sn02: Hz 175 on YzO3: 0 2 984 on A1203: He 383

chemisorption elemental solids molecular

chemisorption structural elemental elemental investigations gases solids molecular on Moo3:

on SO2: on SiOz: Ta 180 HF 569 on CaO: organosilanes 438 Fe 629 on TiOz: Na629 HzO 623 on Zr02: CO 382 Si 678,653 C02 382 on W oxide: organosilanes 435 Ag 723 on Tiz03: HzO 600 on V2O3: HzO 600 on FezO3: H20 600 on ZnO: H20 1193 CO 186 COZ 186 methanol 451 dyes 400

methanol 805 on CaO:

SO2 629 on A1203: HF 569 formic acid 642 propylene 697 aminophenyltrimethoxysilane 350 on BeO: HF 569 on SnOz: propylene 175

Table XIII. Surface Compositional Studies of Metal Oxides compound Si02 PbOz TiOz Ta205 A1203

Ti0 BaO SrO Biz03 wo3

SnO, CaO CUO La oxides Er oxides

ref no.

compound

ref no.

62, 106,401, 901,929, 1105, 1118 747 901, 381,908, 234 901 179, 144,679, 1118 234 875 875

BaPb(l-xlBix03 Cr-doped COO BaTiOa In-doped COO Si02-coated Ti02 MnO, oxides

258

v6°13

213, 1010 1049 875 1059 657 657

VxTicl-x,Oz NiO UOZ Nk.IW03 Nitrided Si02 Ce oxides

46 415 259 477 298 333 1028 1028 613 908 966, 1109 1189 213 1100 657

Table XIV. Surface Structural and Chemisorption Studies of Other Metal Compounds surface structure TiPt3 53 La& 752, 172, 1128 CuCl 1146 Tic 978 Nisi, 178 Pd2Si 1070

elemental gases

chemisorption elemental solids molecular

on Ni silicide: on MoS,: Fe 528 0 2 1082 on MoSz: Ni 528 Hz 310 S 310 0 2 310 on Sic: on WC: Pd 98 0 2 997 on PdzSi: 0 2 154 on NaC1: He 636, 637

on MoS2: CO 310 ethene 1095 on NaC1: fluoromethane 439 on ZnN CO 155 on Cu2S: ethyl xanthate 726 diethyldithiophosphate 725 on P b S xanthate 857

Er203

Er(OHh

are clearly relevant to this section and should also be consulted. X P S studies of the morphology and composition of Pt-black catalysts reduced in aqueous medium and sintered in hydrogen have been reported (821), and the soft X-ray emission spectrum was also studied (8201. Oxygen and nitrogen transitions evolved as a result of increased sintering temperature as well as electron beam irradiation. The effect of a silica substrate on the surface acidity of ruthenium dioxide has been the subject of a recent Fourier transform infrared spectroscopy (FTIR) report in which the effects of carbon monoxide were investigated (977). Copper coverage was monitored with SIMS and XPS in other studies of a bimetallic Cu-Ru system (142). It was found that P d clusters on the surface of ZnO crystals enhance the deh dration rate of ethanol a t low temperatures (506).Nickedased catalysts have been characterized by XPS for properties related to the presence of K (871) and activated carbon (1150). It was shown that spectral intensity ratios can give a quantitative description of finely dispersed nickel particles. In another study of the chemisorption of CO on an alumina catalyst (355),the crystallite size of dispersed NiO was found to be constant up to 8% content loading. Studies of the catalytic activity of other ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985

13QR


Table XV. Surface Composition Studies of Other Metal Compounds compounds MoSi, WSiz Pt silicides Pd silicides Cu silicides Co silicides CUCl FeSz FeS ZrN ErFez ZnCrxq42-x)S* Cu sulfides AgTe, SmSe Sic Tic Ni2N2 ZnSe NaI

ref no.

compounds

28, 771 1071,783,784 1071,402 204,247,251,807, 816,1069,1163, 1070,402 900 860, 164 1145 628 628 155 192 17 1080,1079 983 1006 349 349 273 217 305

MgzSi Ni silicides

ref no.

compound

ref no.

Nb-A1 alloy Ni silicates ZnS TiCL

815 1082,1083 1034 148

NbN PbS Sic

341 148 659

alumina based systems has been reported for interactions with cyclohexane and hydrogen (354) and for metal dispersions of Co and Mo (248). Extensive segregation of Ti and Fe was observed a t 1073 K in an investigation of the interaction between hydro en and samples of Ti-Fe (958). It was determined that t t e hydrogen activity is catalytically activated by the Ti species. Organics. Surface-sensitive techniques continue to find some utility in the characterization of organic materials. XPS and UPS are unanimously the methods of choice, owing to their sensitivity to surface monolayers and freedom from static charge buildup on r electrically conducting specimens. One study of chemical E d i n g at polyimide surfaces has discussed changes in valence and core level spectra caused by annealing and exposure to water (417). Electron stimulated desorption of H+from solid cyclohexane, benzene, and other organics has yielded threshold energies for the ion (543). Desorption cross sections were measured from polymerized methylglutamatic acid and thin films of soap (289). Improved weathering properties for wood following aqueous chromium trioxide treatments of cellulose specimens were found by XPS to correlate with a reduction from the Cr(V1) to Cr(II1) state (1152). EXAFS was used to determine that an iron trichloride dopant in polyacetylene actually exists as iron tetrachloride

Table XVII. Miscellaneous Surface Studies of Other Metal Compounds description

ref no.

electron desorption of alkali ions from alkali halides photon desorption of alkali ions from alkali halides emission characteristics of single-crystal LaBB influence of corrosion on crack growth in A1 alloys effect of O2 and temp on growth of Ti films on steel study of blocking agents for diffusion of A1 into PtSi

854 855 351 1103 1016 716

Table XVIII. Studies of Carbon-Based Materials element


.

elemental gases

1104,546, 135,134 02 1104,1062,440,1061,741 Nz 1104,265 Ar 1104 Kr 1104 Xe 1104,135, 134 Ne 1104 He 383

graphite

109 1071,782, 176, 177, 1073,204,371,773, 1173,277,402,78, 784 498, 153,120 498, 153,120 180,823 823 203, 136 1084 628 7 192 17 1169 963 993 968 490 490 490 968 626

Ti silicides Ti silicides Ta silicides Cr silicides Si,N4 MnS Fe7Ss AIN DvFe, C~C~&(,-~)S~ Ni4Mo LiF MoSez Si-alloyed carbon

Table XVI. Surface Oxidation Studies of Other Metal Compounds compound

ref no.


molecular

other

K 1161,1160,408 HzO 544 Cu 240 Li 408 Rb 408 Cs 408

organics 1025,563,83,1104

carbon films

391

Hz 1185,794 02 874 Nz 874

preparation 1185,1184 fibers 874

diamond

839,829,391

Hz 829, 1185

films 1184,1185

S 450 P 450

coal ~~~~

140 R

ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL I985

organics 450


ion (599).Synchrotron radiation was used in the experiment. A combined AES and SIMS technique was used to study the formation Of amino acid On the surfaces Of Ag, A', Ni, and c u (616). The chemical nature of the metal substrate was found to be important for submonolayer but not for thicker multilayered depositions.

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147R

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Particle Size Analysis Howard G. Barth* and Shao-Tang Sun Hercules Incorporated, Research Center, Wilmington, Delaware 19894

INTRODUCTION Particle size analysis is a specialized area of analytical chemistry which is required in a great number of industries where the product’s end-use is affected by particle size distribution. Particles can be in the form of solids, liquids, (emulsions and dispersions), or gases (bubbles) or an aggregation of molecules as in the case of micelles. In some instances, especially in areas of pharmaceuticals and electronics, analyses are done to ensure the absence of particulate matter. To monitor the environment accurately for particulate matter requires knowing particle size distributions, as well as concentrations, to fully assess health hazards. In view of the growing interest in particle size analysis, especially among analytical chemists, the subject is covered in this issue of Application Reviews. The number of techniques available for particle size analysis is staggering. According to Scarlett (15A),about 400 methods have been reported. Because of the broad scope of this area in terms of techniques and analytical approaches (see Table I), products (see Tables I1 and 111), and size ranges, the authors focused on two major technique areas which have received the most attention in recent years: radiation scattering and chromatographic techniques. These relatively new and growing areas are rapidly becoming techniques of choice especially for the rapid analysis of submicrometer particles. Also included in this review are recent developments involving the more classical techniques listed in Table I as well as a number of related topics (Data Handling and Analysis, Comminution Theory, and Particle Size Generators). Papers published from late 1981 to the end of 1984 (Chemical Abstracts 1982, 96 (1) to 1984 101 (20)) were searched for relevant papers published in English, French, German, and Russian. Polymers in solution were excluded even though they can be classified as particles. Because of the enormous breadth of topics, in terms of sample type, technique, and particle size range, a number of different search strategies were tried in an attempt to include as many pertinent articles as possible. T o this end, we gratefully acknowledge the work of Ruth Curtiss, Hercules Technical Information Division, for her excellent search routines.

GENERAL BOOKS AND REVIEWS During the past several years there has been only a handful of general books on particle characterization. (Books on light scattering are reviewed in the Scatterin section.) By far, the most popular is T. Allen’s book f2A), “Particle Size Measurement”, which is considered the authoritative text on particle size analysis. The book deals in depth with a wide range of topics. Included are chapters on sampling handling,

Table I. Common Particle Size Analysis Techniques

Centrifugal Sedimentation Techniques Disk Centrifuge photosedimentometry Ultracentrifugation Chromatographic Techniques Field-flow fractionation Hydrodynamic chromatography Classification/Collection/SamplingTechniques (mainly for aerosol particles) Cyclone/centrifugal separators Elutriators Impactors

Electrical Sensing Zone Methods (Coulter Principle) Gravitational Sedimentation Techniques Photosedimentometry Microscopy Optical and electron (Image analysis for data processing) Scattering Techniques Classical light scattering (time-averagelight scattering) Doppler anemometry and related velocimetry methods Electric birefringence Fraunhofer diffraction Single-particle counting techniques Neutron scattering Photon correlation spectroscopy (time-dependentlight scattering, quasi-elastic light scattering) Turbidimetry X-ray scattering Sieving/Filtration Surface Area Measurements data treatment and analysis, and on-line particle size analysis. Most particle size analysis techniques are comprehensively treated including sieving, microscopy, gravitational and sedimentation size analysis, centrifugal methods, Coulter principle, light scattering, and surface area and porosity measurements. “Direct Characterization of Fineparticles”, by B. H. Kaye (2A),represents a comprehensive treatment of well-established particle characterization techniques, including sieve fractionation, gravity and centrifugal sedimentation, and elutriation. Also summarized are single particle counting methods. The chapters on particle sampling, image analysis, and particle

0003-27001a510357-15I ~ $ 0 6 . 5 ~ 0 0 1985 American Chemical Society

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Surface characterization - ACS Publications - American Chemical

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