<i>In Situ</i> Investigation of the Early-Stage Growth of Nanoporous Alumina

<div>Anodization of an aluminum layer in phosphoric acid (3 wt%) under a voltage of 90 V. (a) Anodization current versus time (stage II appears around <span class="nowrap"><svg height="8.59436pt" id="M33" style="vertical-align:-0.2455406pt" version="1.1" viewbox="-0.0498162 -8.34882 45.2269 8.59436" width="45.2269pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"><path d="M324 430H196L233 583L223 592L145 529L120 430H54L29 396L31 388H111L56 126C33 15 54 -12 77 -12C137 -12 214 57 250 95L233 119C208 92 155 59 138 59C126 59 120 70 131 125L186 390L298 394L324 430Z"></path></g><g transform="matrix(.013,0,0,-0.013,8.065,0)"><path d="M535 323V373H52V323H535ZM535 138V188H52V138H535Z"></path></g><g transform="matrix(.013,0,0,-0.013,19.328,0)"><path d="M384 0V27C293 34 287 42 287 114V635C232 613 172 594 109 583V559L157 557C201 555 205 550 205 499V114C205 42 199 34 109 27V0H384Z"></path></g><g transform="matrix(.013,0,0,-0.013,25.568,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,31.808,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,40.223,0)"><path d="M319 325C317 349 306 409 297 431C277 440 250 449 209 449C117 449 57 389 57 319C57 243 122 209 182 182C232 159 261 135 261 91C261 48 227 21 190 21C130 21 85 79 68 145L41 140C41 104 51 36 58 22C75 7 121 -12 172 -12C252 -12 337 35 337 126C337 195 286 231 210 262C166 281 126 304 126 348C126 388 152 417 191 417C240 417 274 378 294 318L319 325Z"></path></g></svg>,</span> stage III (pore formation) at around <span class="nowrap"><svg height="8.59436pt" id="M34" style="vertical-align:-0.2455406pt" version="1.1" viewbox="-0.0498162 -8.34882 45.2269 8.59436" width="45.2269pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"><path d="M324 430H196L233 583L223 592L145 529L120 430H54L29 396L31 388H111L56 126C33 15 54 -12 77 -12C137 -12 214 57 250 95L233 119C208 92 155 59 138 59C126 59 120 70 131 125L186 390L298 394L324 430Z"></path></g><g transform="matrix(.013,0,0,-0.013,8.065,0)"><path d="M535 323V373H52V323H535ZM535 138V188H52V138H535Z"></path></g><g transform="matrix(.013,0,0,-0.013,19.328,0)"><path d="M456 178V225H360V632H320C217 496 115 347 20 206V178H280V106C280 40 276 34 189 27V0H445V27C364 34 360 39 360 106V178H456ZM280 225H82C149 335 214 431 278 520H280V225Z"></path></g><g transform="matrix(.013,0,0,-0.013,25.568,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,31.808,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,40.224,0)"><path d="M319 325C317 349 306 409 297 431C277 440 250 449 209 449C117 449 57 389 57 319C57 243 122 209 182 182C232 159 261 135 261 91C261 48 227 21 190 21C130 21 85 79 68 145L41 140C41 104 51 36 58 22C75 7 121 -12 172 -12C252 -12 337 35 337 126C337 195 286 231 210 262C166 281 126 304 126 348C126 388 152 417 191 417C240 417 274 378 294 318L319 325Z"></path></g></svg>,</span> and stage IV (pore propagation) around <svg height="8.59436pt" id="M35" style="vertical-align:-0.2455406pt" version="1.1" viewbox="-0.0498162 -8.34882 51.4903 8.59436" width="51.4903pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"><path d="M324 430H196L233 583L223 592L145 529L120 430H54L29 396L31 388H111L56 126C33 15 54 -12 77 -12C137 -12 214 57 250 95L233 119C208 92 155 59 138 59C126 59 120 70 131 125L186 390L298 394L324 430Z"></path></g><g transform="matrix(.013,0,0,-0.013,8.065,0)"><path d="M535 323V373H52V323H535ZM535 138V188H52V138H535Z"></path></g><g transform="matrix(.013,0,0,-0.013,19.328,0)"><path d="M384 0V27C293 34 287 42 287 114V635C232 613 172 594 109 583V559L157 557C201 555 205 550 205 499V114C205 42 199 34 109 27V0H384Z"></path></g><g transform="matrix(.013,0,0,-0.013,25.568,0)"><path d="M447 623H65C61 580 56 530 47 475H76C100 541 106 550 172 550H388C308 376 196 170 91 -1L98 -12L172 -2C268 204 360 408 455 611L447 623Z"></path></g><g transform="matrix(.013,0,0,-0.013,31.81,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,38.05,0)"><path d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"></path></g><g transform="matrix(.013,0,0,-0.013,46.465,0)"><path d="M319 325C317 349 306 409 297 431C277 440 250 449 209 449C117 449 57 389 57 319C57 243 122 209 182 182C232 159 261 135 261 91C261 48 227 21 190 21C130 21 85 79 68 145L41 140C41 104 51 36 58 22C75 7 121 -12 172 -12C252 -12 337 35 337 126C337 195 286 231 210 262C166 281 126 304 126 348C126 388 152 417 191 417C240 417 274 378 294 318L319 325Z"></path></g></svg>). (b) Integrated intensity along the <svg height="11.4899pt" id="M36" style="vertical-align:-5.52899pt" version="1.1" viewbox="-0.0498162 -5.96091 12.3012 11.4899" width="12.3012pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"><path d="M474 429L457 433C435 440 389 448 367 448C348 448 323 446 309 443C266 434 195 406 148 366C78 307 23 210 23 101C23 35 55 -12 92 -12C118 -12 146 1 196 35C247 70 311 130 346 173H348L281 -148C268 -211 256 -221 208 -229L191 -232L187 -257L433 -245L437 -219L411 -216C357 -210 350 -205 362 -140L427 207C447 315 461 381 474 429ZM387 387C379 337 363 262 355 236C318 180 201 57 142 57C126 57 112 81 112 128C112 205 150 321 220 376C244 395 280 403 312 403C345 403 370 396 387 387Z"></path></g><g transform="matrix(.0091,0,0,-0.0091,6.318,3.132)"><path d="M563 395C563 428 543 451 519 451C500 451 480 438 472 423C468 415 465 403 470 394C477 381 482 368 482 347C482 272 386 136 342 74H340C334 163 323 257 312 337C302 410 290 451 257 451C214 451 160 385 127 338L145 310C169 341 203 373 209 373C219 373 225 369 232 325C249 215 269 62 271 -15C220 -80 135 -165 18 -231L26 -257L142 -230C254 -105 279 -74 342 13C394 85 484 211 526 286C553 334 563 365 563 395Z"></path></g></svg> axis and full width at half maximum (along <svg height="11.4899pt" id="M37" style="vertical-align:-5.52899pt" version="1.1" viewbox="-0.0498162 -5.96091 12.3012 11.4899" width="12.3012pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"><path d="M474 429L457 433C435 440 389 448 367 448C348 448 323 446 309 443C266 434 195 406 148 366C78 307 23 210 23 101C23 35 55 -12 92 -12C118 -12 146 1 196 35C247 70 311 130 346 173H348L281 -148C268 -211 256 -221 208 -229L191 -232L187 -257L433 -245L437 -219L411 -216C357 -210 350 -205 362 -140L427 207C447 315 461 381 474 429ZM387 387C379 337 363 262 355 236C318 180 201 57 142 57C126 57 112 81 112 128C112 205 150 321 220 376C244 395 280 403 312 403C345 403 370 396 387 387Z"></path></g><g transform="matrix(.0091,0,0,-0.0091,6.318,3.132)"><path d="M563 395C563 428 543 451 519 451C500 451 480 438 472 423C468 415 465 403 470 394C477 381 482 368 482 347C482 272 386 136 342 74H340C334 163 323 257 312 337C302 410 290 451 257 451C214 451 160 385 127 338L145 310C169 341 203 373 209 373C219 373 225 369 232 325C249 215 269 62 271 -15C220 -80 135 -165 18 -231L26 -257L142 -230C254 -105 279 -74 342 13C394 85 484 211 526 286C553 334 563 365 563 395Z"></path></g></svg> axis) as a function of the anodizing time.</div>

Journal of Nanomaterials

fig4

Figure 4

Figure 4: <i>In Situ</i> Investigation of the Early-Stage Growth of Nanoporous Alumina 

Journal of Nanomaterials

In Situ Investigation of the Early-Stage Growth of Nanoporous Alumina

Figure 4