Name: metal-assisted electrochemical nanoimprinting of porous and solid silicon wafers
Uploaded: 2022-02-08T12:30:00
Description: Watch this Scientific Journal Video about Metal-Assisted Electrochemical Nanoimprinting of Porous and Solid Silicon Wafers at JoVE.com

Vi anerkender Dr. Keng Hsu (University of Louisville) for indsigt i dette arbejde; Frederick Seitz Laboratory fra University of Illinois og i memoriam ansat Scott Maclaren; Arizona State University's LeRoy Eyring Center for Solid State Science; og Science Foundation Arizona under Bis grove Scholars Award.

FORSIGTIG: Brug passende sikkerhedspraksis og personlige værnemidler (f.eks. kittel, handsker, sikkerhedsbriller, lukkede sko). Denne procedure anvender HF syre (48% wt), som er en yderst farlig kemisk og kræver yderligere personlige værnemidler (dvs. et ansigt skjold, naturlige gummi forklæde, og andet par nitril handsker, der dækker hånd, håndled, og underarme).
1. Stempelforberedelse til Mac-aftryk
<ol><li>
PDMS skimmel fabrikation
	<ol>
<li>RCA-1 opløsningen til ...

<ol>
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C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanotextured+Silica+Surfaces+with+Robust+Superhydrophobicity+and+Omnidirectional+Broadband+Supertransmissivity.">Nanotextured Silica Surfaces with Robust Superhydrophobicity and Omnidirectional Broadband Supertransmissivity.</a> ACS Nano. 6 (5), 3789-3799 (2012).</li><li>Kim, J., Joy, D. C., Lee, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Controlling+resist+thickness+and+etch+depth+for+fabrication+of+3D+structures+in+electron-beam+grayscale+lithography.">Controlling resist thickness and etch depth for fabrication of 3D structures in electron-beam grayscale lithography.</a> Microelectronics Engineering. 84 (12), 2859-2864 (2007).</li><li>Deng, S., Zhang, Y., Jiang, S., Lu, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+of+three-dimensional+silicon+structure+with+smooth+curved+surfaces.">Fabrication of three-dimensional silicon structure with smooth curved surfaces.</a> Journal of Micro/Nanolithography, MEMS, and MOEMS. 15 (3), 0345031-0345036 (2016).</li><li>Azeredo, B. P., Lin, Y., Avagyan, A., Sivaguru, M., Hsu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Imprinting+of+Porous+Silicon+via+Metal-Assisted+Chemical+Etching.">Direct Imprinting of Porous Silicon via Metal-Assisted Chemical Etching.</a> Advanced Functional Materials. 26 (17), 2929-2939 (2016).</li><li>Azeredo, B., Hsu, K., Ferreira, P. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Electrochemical+Imprinting+of+Sinusoidal+Linear+Gratings+into+Silicon.">Direct Electrochemical Imprinting of Sinusoidal Linear Gratings into Silicon.</a> The American Society of Mechanical Engineers - International Manufacturing Science and Engineering Conference. , 1-6 (2016).</li><li>Li, H., Niu, J., Wang, G., Wang, E., Xie, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Production+of+Silicon+Nanostructures+with+Electrochemical+Nanoimprinting.">Direct Production of Silicon Nanostructures with Electrochemical Nanoimprinting.</a> ACS Applied Electronic Materials. 1 (7), 1070-1075 (2019).</li><li>Kim, K., Ki, B., Choi, K., Lee, S., Oh, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resist-Free+Direct+Stamp+Imprinting+of+GaAs+via+Metal-Assisted+Chemical+Etching.">Resist-Free Direct Stamp Imprinting of GaAs via Metal-Assisted Chemical Etching.</a> ACS Applied Materials &amp; Interfaces. 11 (14), 13574-13580 (2019).</li><li>Zhang, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Contact+electrification+induced+interfacial+reactions+and+direct+electrochemical+nanoimprint+lithography+in+n-type+gallium+arsenate+wafer.">Contact electrification induced interfacial reactions and direct electrochemical nanoimprint lithography in n-type gallium arsenate wafer.</a> Chemical Science. 8, 2407-2412 (2017).</li><li>Zhan, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+micro/nano-machining:+principles+and+practices.">Electrochemical micro/nano-machining: principles and practices.</a> Chemical Society Reviews. 46 (5), 1526-1544 (2017).</li><li>Li, X., Bohn, P. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Metal-assisted+chemical+etching+in+HF+/+H2O2+produces+porous+silicon.">Metal-assisted chemical etching in HF / H2O2 produces porous silicon.</a> Applied Physics Letters. 77 (16), 2572-2574 (2000).</li><li>Chartier, C., Bastide, S., Levy-Clement, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Metal-assisted+chemical+etching+of+silicon+in+HF+-+H2O2.">Metal-assisted chemical etching of silicon in HF - H2O2.</a> Electrochimica Acta. 53, 5509-5516 (2008).</li><li>Chattopadhyay, S., Li, X., Bohn, P. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In-plane+control+of+morphology+and+tunable+photoluminescence+in+porous+silicon+produced+by+metal-assisted+electroless+chemical+etching.">In-plane control of morphology and tunable photoluminescence in porous silicon produced by metal-assisted electroless chemical etching.</a> Journal of Applied Physics. 91 (9), 6134-6140 (2002).</li><li>Torralba, E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=3D+patterning+of+silicon+by+contact+etching+with+anodically+biased+nanoporous+gold+electrodes.">3D patterning of silicon by contact etching with anodically biased nanoporous gold electrodes.</a> Electrochemistry Communications. 76, 79-82 (2017).</li><li>Bastide, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=3D+Patterning+of+Si+by+Contact+Etching+With+Nanoporous+Metals.">3D Patterning of Si by Contact Etching With Nanoporous Metals.</a> Frontiers in Chemistry. 7, 1-13 (2019).</li><li>Sharstniou, A., Niauzorau, S., Ferreira, P. M., Azeredo, B. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+nanoimprinting+of+silicon.">Electrochemical nanoimprinting of silicon.</a> Proceedings of the National Academy of Sciences. 116 (21), 10264-10269 (2019).</li><li>Niauzorau, S., Ferreira, P., Azeredo, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+Porous+Noble+Metal+Films+with+Tunable+Porosity+by+Timed+Dealloying.">Synthesis of Porous Noble Metal Films with Tunable Porosity by Timed Dealloying.</a> The American Society of Mechanical Engineers - International Manufacturing Science and Engineering Conference. , 1-4 (2018).</li><li>Geyer, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Model+for+the+Mass+Transport+During+Metal-Assisted+Chemical+Etching+with+Contiguous+Metal+Films+As+Catalysts.">Model for the Mass Transport During Metal-Assisted Chemical Etching with Contiguous Metal Films As Catalysts.</a> The Journal of Physical Chemistry C. 116 (24), 13446-13451 (2012).</li><li>Li, L., Liu, Y., Zhao, X., Lin, Z., Wong, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Uniform+Vertical+Trench+Etching+on+Silicon+with+High+Aspect+Ratio+by+Metal-Assisted+Chemical+Etching+Using+Nanoporous+Catalysts.">Uniform Vertical Trench Etching on Silicon with High Aspect Ratio by Metal-Assisted Chemical Etching Using Nanoporous Catalysts.</a> ACS Applied Materials and Interfaces. 6 (1), 575-584 (2014).</li></ol>

Mac-Aftryksfrimærker og forlagte Si-chips (p-type, [100] orientering, 1-10 Ohm∙cm) blev udarbejdet i henhold til henholdsvis protokollens afsnit 1 og 2. Mac-aftrykket af prepatterned Si-chip med frimærker, der indeholder 3D-hierarkiske mønstre, blev udført i henhold til protokollens afsnit 3 (figur 9). Som vist i figur 9a blev der anvendt forskellige konfigurationer af Mac-aftryk: solid Si med solid Au (venstre), porøs Si med solid Au (mi...

Tredimensionelle mikro- og nanoskalamønstre og teksturering af halvledere muliggør mange anvendelser på forskellige områder, såsom optoelektronik1,2, fotonik3, antireflektive overflader4, super hydrofobiske og selvrensende overflader5,6 blandt andre. Prototyping og masseproducerende 3D og hierarkiske mønstre er med succes blevet udført for polymere film ved blød litografi og nanoimprinting litografi med sub-20 nm opløsning. Overførsel af sådanne 3D polymere mønstre til Si kræver imidlertid den ætsende selektivitet af et maskemønster under reaktiv ion ætsning og begrænser dermed billedformatet og fremkalder formforvrængninger og overflade ruhed på grund af flossede virkninger7,8.
En ny metode kaldet Mac-Aftryk er opnået for parallel og direkte mønstre af porøse9 og faste Si wafers10,11 samt solid GaAs wafers12,13,14. Mac-Imprint er en kontaktbaseret våd ætsning teknik, der kræver kontakt mellem substrat og en ædel metal-belagt stempel besidder 3D-funktioner i nærværelse af en ætsning løsning (ES) bestående af HF og en oxidant (f.eks H2O2 i tilfælde af Si Mac-Aftryk). Under ætsningen forekommer to reaktioner samtidigt15,16: en katodisk reaktion (dvs. H2O2-reduktionen ved ædelmetal, hvor der genereres positive ladebærere [huller] og efterfølgende injiceres i Si17) og en anodisk reaktion (dvs. Si opløsning, hvor hullerne forbruges). Efter tilstrækkelig kontakt ætses stemplets 3D-funktioner ind i Si wafer. Mac-Imprint har mange fordele i forhold til konventionelle litografiske metoder, såsom høj gennemløb, kompatibilitet med roll-to-plate og roll-to-roll platforme, amorfe, mono- og polykrystallin Si og III-V halvledere. Mac-aftryksstempler kan genbruges flere gange. Derudover kan metoden levere en sub-20 nm ætsning opløsning, der er kompatibel med moderne direkte skrivemetoder.
Nøglen til at opnå high-fidelity prægning er diffusion vej til ætsning front (dvs. kontakt interface mellem katalysator og substrat). Arbejdet i Azeredo et al.9 viste først, at ES diffusion er aktiveret gennem et porøst Si-netværk. Torralba et al.18, rapporterede, at for at realisere solid Si Mac-Aftryk ES diffusion er aktiveret gennem en porøs katalysator. Bastide et al.19 og Sharstniou et al.20 undersøgte yderligere katalysator porositeten indflydelse på ES diffusion. Således er begrebet Mac-Imprint blevet testet i tre konfigurationer med forskellige diffusionsveje.
I den første konfiguration er katalysatoren og substratet solid, hvilket ikke giver nogen indledende diffusionsvej. Manglen på reaktiv diffusion fører til en sekundær reaktion under prægning, der danner et lag af porøs Si på substratet omkring kanten af katalysator-Si interface. Reaktanterne er efterfølgende udtømt, og reaktionen stopper, hvilket resulterer i ingen mærkbar mønsteroverførsels troskab mellem stemplet og substratet. I den anden og tredje konfiguration aktiveres diffusionsvejene gennem porøse netværk, der indføres enten i substratet (dvs. porøse Si) eller i katalysatoren (dvs. porøst guld), og der opnås høj mønsteroverførselsnøjagtighed. Massetransporten gennem porøse materialer spiller således en afgørende rolle med hensyn til at muliggøre spredning af reaktanter og reaktionsprodukter til og fra kontaktgrænsefladen9,18,19,20. Et skema over alle tre konfigurationer vises i figur 1.
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/61040/61040fig1.jpg"> Figur 1: Skemaer over Mac-aftrykskonfigurationer. Dette tal fremhæver porøse materialers rolle med hensyn til at muliggøre diffusion af reagerende arter gennem substratet (dvs. sag II: porøse Si) eller i stemplet (dvs. sag III: katalysatortynd film lavet af porøs guld). <a href="https://www.jove.com/files/ftp_upload/61040/61040fig1large.jpg" target="_blank">Klik her for at se en større version af dette tal.</a>
I dette papir diskuteres Mac-Imprint-processen grundigt, herunder stempelforberedelse og substratforbehandling sammen med Mac-Imprint selv. Substratforbehandlingsafsnittet i protokollen omfatter si waferrensning og si wafermønstre med tør ætsning og substrat anodisering (valgfrit). Endvidere er et stempel forberedelse sektion opdelt i flere procedurer: 1) PDMS replika støbning af Si master skimmel; 2) UV nanoimprinting af et fotoresistlag med henblik på at overføre PDMS-mønsteret og 3) katalytisk lagaflejring via magnetron sputtering efterfulgt af dealloying (valgfrit). Endelig præsenteres Mac-Imprint-opsætningen i Mac-Imprint-opsætningen sammen med Mac-Imprint-resultaterne (dvs. Si-overflade 3D-hierarkisk mønster).

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	<tbody>
		<tr>
			<td>Acetone, &#62;99.5%, ACS reagent</td>
			<td>Sigma-Aldrich</td>
			<td>67-64-1</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>Ammonium fluoride, &#62;98%, ACS grade</td>
			<td>Sigma-Aldrich</td>
			<td>12125-01-8</td>
			<td>CAUTION, hazardous</td>
		</tr>
		<tr>
			<td>Ammonium hydroxide solution, 28-30%, ACS reagent</td>
			<td>Sigma-Aldrich</td>
			<td>1336-21-6</td>
			<td>CAUTION, hazardous</td>
		</tr>
		<tr>
			<td>AZ 400K developer</td>
			<td>Microchemicals</td>
			<td>AZ 400K</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>BenchMark 800 Etch</td>
			<td>Axic</td>
			<td>BenchMark 800</td>
			<td>Reactive ion etching</td>
		</tr>
		<tr>
			<td>Chromium target, 2&#34; x 0.125&#34;, 99.95% purity</td>
			<td>ACI alloys</td>
			<td>ADM0913</td>
			<td>Magnetron sputter chromium target</td>
		</tr>
		<tr>
			<td>CTF 12</td>
			<td>Carbolite Gero</td>
			<td>C12075-700-208SN</td>
			<td>Tube furnace</td>
		</tr>
		<tr>
			<td>Desiccator</td>
			<td>Fisher scientific Chemglass life sciences</td>
			<td>CG122611</td>
			<td>Desiccator</td>
		</tr>
		<tr>
			<td>F6T5/BLB</td>
			<td>Eiko</td>
			<td>F6T5/BLB 6W</td>
			<td>UV bulb</td>
		</tr>
		<tr>
			<td>Gold target, 2&#34; x 0.125&#34;, 99.99% purity</td>
			<td>ACI alloys</td>
			<td>N/A</td>
			<td>Magnetron sputter gold target</td>
		</tr>
		<tr>
			<td>Hotplate KW-4AH</td>
			<td>Chemat tecnologie</td>
			<td>KW-4AH</td>
			<td>Leveled hotplate with uniform temperature profile</td>
		</tr>
		<tr>
			<td>Hydrofluoric acid, 48%, ACS reagent</td>
			<td>Sigma-Aldrich</td>
			<td>7664-39-3</td>
			<td>CAUTION, extremly hazardous</td>
		</tr>
		<tr>
			<td>Hydrogen peroxide, 30%, ACS reagent</td>
			<td>Fisher Chemical</td>
			<td>7722-84-1</td>
			<td>CAUTION, hazardous</td>
		</tr>
		<tr>
			<td>Isopropyl alcohol, &#62;99.5%, ACS reagent</td>
			<td>LabChem</td>
			<td>67-63-0</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>MLP-50</td>
			<td>Transducer Techniques</td>
			<td>MLP-50</td>
			<td>Load cell</td>
		</tr>
		<tr>
			<td>Nitric acid, 70%, ACS grade</td>
			<td>SAFC</td>
			<td>7697-37-2</td>
			<td>CAUTION, hazardous</td>
		</tr>
		<tr>
			<td>NSC-3000</td>
			<td>Nano-master</td>
			<td>NSC-3000</td>
			<td>Magnetron sputter</td>
		</tr>
		<tr>
			<td>Potassium hydroxide, 45%, Certified</td>
			<td>Fisher Chemical</td>
			<td>1310-58-3</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>Rocker 800 vacuum pump, 110V/60Hz</td>
			<td>Rocker</td>
			<td>1240043</td>
			<td>Oil-free vacuum pump</td>
		</tr>
		<tr>
			<td>Silicon master mold</td>
			<td>NILT</td>
			<td>SMLA_V1</td>
			<td>Silicon chip with pattern</td>
		</tr>
		<tr>
			<td>Silicon wafers, prime grade</td>
			<td>University wafer</td>
			<td>783</td>
			<td>Si wafer</td>
		</tr>
		<tr>
			<td>Silver target, 2&#34; x 0.125&#34;, 99.99% purity</td>
			<td>ACI alloys</td>
			<td>HER2318</td>
			<td>Magnetron sputter silver target</td>
		</tr>
		<tr>
			<td>SP-300</td>
			<td>BioLogic</td>
			<td>SP-300</td>
			<td>Potentiostat</td>
		</tr>
		<tr>
			<td>SPIN 150i</td>
			<td>Spincoating</td>
			<td>SPIN 150i</td>
			<td>Spin coater</td>
		</tr>
		<tr>
			<td>SPR 200-7.0 positive photoresist</td>
			<td>Microchem</td>
			<td>SPR 220-7.0</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>Stirring hotplate</td>
			<td>Thermo scientific Cimarec+</td>
			<td>SP88857100</td>
			<td>General purpose hotplate</td>
		</tr>
		<tr>
			<td>SU-8 2015 negative photoresist</td>
			<td>Microchem</td>
			<td>SU-8 2015</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>SYLGARD 184 Silicone elastomere kit</td>
			<td>DOW</td>
			<td>4019862</td>
			<td>CAUTION, chemical</td>
		</tr>
		<tr>
			<td>T-LSR150B</td>
			<td>Zaber Technologies</td>
			<td>T-LSR150B-KT04U</td>
			<td>Motorized linear stage</td>
		</tr>
		<tr>
			<td>Trichloro(1H,1H,2H,2H-perfluorooctyl)silane (PFOCS), 97%</td>
			<td>Sigma-Aldrich</td>
			<td>78560-45-9</td>
			<td>CAUTION, hazardous</td>
		</tr>
	</tbody>
</table>

metal-assisted electrochemical nanoimprinting of porous and solid silicon wafers

Metalassisteret elektrokemisk prægning (Mac-Aftryk) er en kombination af metalassisteret kemisk ætsning (MACE) og nanoimprint litografi, der er i stand til direkte at mønstre 3D mikro- og nanoskalafunktioner i monokrystallinsk gruppe IV (f.eks. Si) og III-V (f.eks. GaAs) halvledere uden behov for offerskabeloner og litografiske trin. Under denne proces bringes et genanvendeligt stempel belagt med en ædelmetalkatalysator i kontakt med en Si wafer i nærværelse af en hydrofluorsyre (HF) og hydrogenperoxid (H2O2) blanding, hvilket fører til selektiv ætsning af Si ved metal-halvlederkontaktgrænsefladen. I denne protokol diskuterer vi de stempel- og substratforberedelsesmetoder, der anvendes i to Mac-Imprint-konfigurationer: (1) Porous Si Mac-Aftryk med en solid katalysator; og (2) Solid Si Mac-aftryk med en porøs katalysator. Denne proces er høj gennemløb og er i stand til centimeter-skala parallel mønstre med sub-20 nm opløsning. Det giver også lav defekt densitet og store areal mønstre i en enkelt operation og omgår behovet for tør ætsning såsom dyb reaktiv ion ætsning (DRIE).

Scanning elektron mikroskop (SEM) billeder, optiske mikroskop scanninger (Figur 9), og atomprøvesprængninger (AFM) scanninger (Figur 10) blev opnået for at studere morfologiske egenskaber mac-aftryk frimærker og påtrykt Si overflader. Den tværsnitsprofil af det påtrykte faste Si blev sammenlignet med den anvendte porøse Au-stempel (figur 10). Mønsteroverførsels troskab og porøs Si-generati...

Watch this Scientific Journal Video about Metal-Assisted Electrochemical Nanoimprinting of Porous and Solid Silicon Wafers at JoVE.com

Metal-Assisted Electrochemical Nanoimprinting of Porous and Solid Silicon Wafers

En protokol for metal-assisteret kemisk prægning af 3D mikroskala funktioner med sub-20 nm form nøjagtighed i faste og porøse silicium wafers præsenteres.

Metalassisteret elektrokemisk nanoimprinting af porøse og faste silicium wafere

Metal-assisted electrochemical imprinting (Mac-Imprint) is a combination of metal-assisted chemical etching (MACE) and nanoimprint lithography that is ...

Vores protokol giver en ny mønstremetode til silicium, der gør det muligt at skabe tredimensionelle hierarkiske mikrostrukturer, der muliggør design af metaoverfladebaserede mikrooptiske elementer og bølgelederteknologier. Denne protokol giver mulighed for replikation af 3D-strukturer fra polymere og hårde forme til monokrystallinske og porøse silicium wafers i et enkelt trin. Og samtidig giver sub 100 nanometer opløsninger i alle tre retninger.Porøs silicium og silicium i sig selv er gode materialer til fremstilling af optiske biosensorer og infrarøde optiske enheder. Vi forventer dog, at denne teknik udvides til gruppen III-V halvledere og endda videre. Stempel til substrat tip og hældning justering er yderst vigtigt for en ensartet Mac-aftryk.Efter denne protokol kan justeringen udføres ved monteringsstempel til holderen, mens den er i kontakt med substratet. For at forberede et stempel til Mac-aftrykket skal du først rengøre siliciummasterformen ved hjælp af RCA-1-opløsning i henhold til de trin, der er beskrevet i protokollen, og derefter placere en ren siliciummasterform i en plastik petriskål inde i en udtørrer. Brug en plastikpipette til at tilføje et par dråber PFOCS til en plastvægtbåd og placere vejebåden ved siden af skålen med mesterformen.Tænd vakuumpumpen, åbn udsikkatorventilen, og anfør vakuum i 30 minutter. Mens vakuumet påføres, skal du bruge en glasspatel til at blande basen og hærdemidlet fra et silicium elastomersæt i et 10-til-en-forhold i 10 til 15 minutter. I slutningen af udtørring, fjerne veje båd fra udtørrer og afstandsfly fra under silicium master skimmel, derefter omhyggeligt dække master skimmel med en to til tre millimeter lag af frisklavede PDMS.Hvis du vil afgas PDMS efter åbning af udtørrerventilen, skal der påføres vakuum i yderligere 20 minutter, eller indtil boblerne forsvinder. I slutningen af den anden udtørringsperiode overføres skålen til en 80 grader Celsius kogeplade. Efter to timer skal du bruge en skalpel til at trimme kanterne af den hærdede PDMS inde i plast Petriskål og bruge pincet til forsigtigt at fjerne PDMS skimmelsvamp fra silicium master skimmel.For fotoresist UV nanoimprinting, skal du bruge en skriver til at kløve en 2,5 gange 2,5 centimeter silicium chip ud af silicium wafer, rengøring det ved hjælp af RCA-1 løsning i henhold til de trin, der er beskrevet i protokollen og derefter placere den rene chip på vakuum i en spin coater. Indstil spin coating parametre som angivet til at anvende en 20 mikrometer tyk lag fotoresist på chippen og tryk VAC ON at anvende vakuum på systemet. Hæld 1,5 milliliter SU-8 2015 fotoresist på midten af chippen og luk spin coater låget.Tryk derefter på Start for at starte spin. I slutningen af spin, tryk på VAC OFF for at slukke for vakuum og bruge pincet til at fjerne fotoresist-belagt chip. Placer forsigtigt PDMS-formen på det fotoresistbelagte siliciumchipmønster side ned og tryk manuelt formen ind i chippen.Placer en UV gennemsigtig glasplade oven på PDMS til at anvende 15 gram pr kvadratcentimeter af tryk på formen og chip og udsætte opsætningen til seks watt UV-lys i to timer. I slutningen af bestrålingsperioden skal du bruge pincet til langsomt at fjerne formen fra chippen i retning parallelt med retningen af det hærdede fotoresistmønster. For at deponere et 250 nanometer tykt guld / sølvlegeringslag på chippen, skal du først deponere 20 nanometer tykt lag krom og 50 nanometer tykt lag guld, som det er beskrevet i tekstprotokollen.Klik derefter på GUN 1 OPEN for at åbne lukkeren for guld- og sølvpistolen. Indstil tiden til at behandle til 16,5 minutter, og indstil DC-sættepunktet til 58 og RF-sættepunktet til 150. Klik på Rotation, og angiv argonflowhastigheden til 50 kubikcentimeter i minuttet.Klik på Argon, DC Supply og RF Supply. Når signalet plateauer, indstille argon control til fem. Klik på Start i nultykkelse for at starte henholdsvis krystaltykkelsen og rive tykkelsen i stykker.Klik på Tid tid tid til at starte den tidsstyrede proces og klikke på PLATEN SHUTTER Solid for at åbne pladeskodderen. Klik på nul tykkelse igen. Når sputtering slutter, skal du klikke på Fast for at lukke pladens faste lukker og tryk på Tryk for at udlufte magnetron sputterkammeret.For at de-legering sølv / guldlegering belagt Mac-aftryk stempel, først blande deioniseret vand og salpetersyre på en en-til-en forhold i et glas bægerglas og placere bægerglasset på en omrøring kogeplade. Dyk ned en perforeret PTFE prøveholder i blandingen og opvarme opløsningen op til 65 grader Celsius med konstant omrøring ved 100 omdrejninger i minuttet. Når opløsningen har nået måltemperaturen, skal du placere det mønstrede sølv/sølvlegeringsbelagte Mac-aftryksstempel i holderen i to til 20 minutter.Efter de-legering, slukke Mac-aftryk stempel i stuetemperatur deioniseret vand i et minut. For at udføre stempel til substratjustering skal du placere stemplet nedad på toppen af siliciumchip i elektrokemisk celle, tilføje en dråbe SU-8 på bagsiden af stemplet. Bring PTFE stang i kontakt med SU-8 og helbrede det på plads under tørre forhold under UV-lys i to timer.Kontakten er omkring 86 millimeter fra hjemmet position. For at udføre en Mac-prægning operation, ren mønstret silicium chip ved hjælp af RCA løsning i henhold til de trin, der er beskrevet i protokollen og derefter placere den i midten af en elektrokemisk celle og placere cellen under en PTFE stang med Mac-aftryk stempel. Bland ætsningsopløsningen af flussyre og brintoverilte i et 17-til-en-forhold inde i et PTFE-bægerglas.Efter fem minutter skal du bruge en plastpipette til at tilføje ætsningsopløsningen til den elektrokemiske celle. For at placere Mac-aftrykket stempel i kontakt med mønster chip, bringe stemplet ned med omkring 86 millimeter og derefter flytte stemplet ned fra kontaktpositionen med omkring 300 til 1.000 mikrometer for at opnå den ønskede kontakt kraft. Bevar Mac-aftrykket stempel i kontakt med chippen fra en til 30 minutter, før du klikker hjem for at returnere stangen til hjemmet position.Brug en pipette til forsigtigt at aspirere ætsningsopløsningen fra cellen og skyl den påtrykte siliciumchip med isopropylalkohol og deioniseret vand. Tør derefter chippen med ren tør luft. Scanning elektron mikroskop billeder kan fås til at studere morfologiske egenskaber af guldbelagte Mac-aftryk frimærker og den deraf følgende påtrykte silicium overflader.I denne repræsentative analyse blev tværsnitsprofilen af det påtrykte faste silicium, der blev opnået ved atomprøvesprængning, sammenlignet med det anvendte porøse guldstempel. Mønsteroverførsels troskab og porøs siliciumgenerering under Mac-aftryk var to store kriterier for at analysere den eksperimentelle succes. Mac-aftrykket blev betragtet som vellykket, hvis frimærkemønsteret blev nøjagtigt overført til silicium, og der ikke blev genereret porøst silicium under Mac-aftrykket.Her kan resultaterne af et suboptimalt eksperiment, hvor der opstod mangel på mønsteroverførsels troskab og en porøs siliciumgeneration under Mac-aftrykket. Det er vigtigt at huske, at Mac-aftryk af silicium involverer flussyre, som er livstruende stof og efter en sikkerhedsprotokol og iført passende personlige værnemidler er altafgørende. Når du bruger frimærker belagt med porøst guld for at lette massetransport.Efter denne procedure kan sammensætningen af ætsningsopløsningen eller kontaktkraften varieres for at studere processens kineti eller stempel holdbarheden.

metal-assisted-electrochemical-nanoimprinting-porous-solid-silicon

Research

JoVE Journal

Engineering

Nanomoulding of Functional Materials, a Versatile Complementary Pattern Replication Method to Nanoimprinting

We describe a nanomoulding technique which allows low-cost nanoscale patterning of functional materials, materials stacks and full devices. Nanomoulding combined with layer transfer enables the replication of arbitrary surface patterns from a master structure onto the functional material. Nanomoulding can be performed on any nanoimprinting setup and can be applied to a wide range of materials and deposition processes. In particular we demonstrate the fabrication of patterned transparent zinc oxide electrodes for light trapping applications in solar cells.

We describe a nanomoulding technique which allows low-cost nanoscale patterning of functional materials, materials stacks and full devices. Nanomoulding can be performed on any nanoimprinting setup and can be applied to a wide range of materials and deposition processes.

Nanomoulding af funktionelle materialer, en alsidig komplementært mønster Replication Metode til Nanoimprinting

We describe a nanomoulding technique which  allows low-cost nanoscale patterning of functional materials, materials stacks  and full devices. Nanomoulding ...

Fabrication of VB2/Air Cells for Electrochemical Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for synthesizing nanoscopic VB2 is presented as well as step-by-step procedure for applying a zirconium oxide coating to the VB2 particles for stabilization upon discharge. The process for disassembling existing zinc/air cells is shown, in addition construction of the new working electrode to replace the conventional zinc/air cell anode with a the nanoscopic VB2 anode. Finally, discharge of the completed VB2/air battery is reported. We show that using the zinc/air cell as a test bed is useful to provide a consistent configuration to study the performance of the high-energy high capacity nanoscopic VB2 anode.

Fabrication of VB2/Air Cells for Electrochemical Testing

A protocol is presented to study multi-electron metal/air battery systems by using previous technology developed for the zinc/air cell. Electrochemical testing is then performed on fabricated batteries to evaluate performance.

Fabrikation af VB<sub&gt; 2</sub&gt; / Air Celler til Elektrokemisk Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for ...

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

Enkeltlags Kontakt doping af silicium overflader og nanotråde Brug organophosphorforbindelser

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned and bonded silicon wafers. Unlike confinements in porous materials often used for these types of experiments3, bonded wafers provide predesigned uniform spaces for confinement. The geometry of each cell is well known, which removes a large source of ambiguity in the interpretation of data.
Exceptionally flat, 5 cm diameter, 375 &#181;m thick Si wafers with about 1 &#181;m variation over the entire wafer can be obtained commercially (from Semiconductor Processing Company, for example). Thermal oxide is grown on the wafers to define the confinement dimension in the z-direction. A pattern is then etched in the oxide using lithographic techniques so as to create a desired enclosure upon bonding. A hole is drilled in one of the wafers (the top) to allow for the introduction of the liquid to be measured. The wafers are cleaned2 in RCA solutions and then put in a microclean chamber where they are rinsed with deionized water4. The wafers are bonded at RT and then annealed at ~1,100 &#176;C. This forms a strong and permanent bond. This process can be used to make uniform enclosures for measuring thermal and hydrodynamic properties of confined liquids from the nanometer to the micrometer scale.

A method for permanently bonding two silicon wafers so as to realize a uniform enclosure is described. This includes wafer preparation, cleaning, RT bonding, and annealing processes. The resulting bonded wafers (cells) have uniformity of enclosure ~1%1,2. The resulting geometry allows for measurements of confined liquids and gasses.

Fremstilling af ensartede nanoskala hulrum via Silicon Direct Wafer Bonding

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

Protokol for elektrokemisk Test og karakterisering på aprotiske Li-O<sub&gt; 2</sub&gt; Batteri

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Spektroskopisk Boundary Layer Undersøgelse under ablative Material Testing i PlasmaTron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. The results of studies in which the etching current and the molarity of the NaOH solution used in the etching process were varied are presented. The investigation of the geometry of the tips, by imaging them with a scanning electron microscope, and by operating them in field emission mode is also described. The field emission tips produced are intended to be used as an electron beam source for ion production via electron impact ionization of background gas or vapor in Penning trap mass spectrometry applications.

A method for electrochemically etching field emission tips is presented. Etching parameters are characterized and the operation of the tips in field emission mode is investigated.

Elektrokemisk Ætsning og karakterisering af Sharp Field Emission Point for Electron Impact ionisering

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. ...

Fabrication of White Light-emitting Electrochemical Cells with Stable Emission from Exciplexes

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active layer which consists of blue-fluorescent poly(9,9-di-n-dodecylfluorenyl-2,7-diyl) (PFD) and &#960;-conjugated triphenylamine molecules. This white light emission originates from exciplexes formed between PFD and amines in electronically excited states. A device containing PFD, 4,4&#39;,4&#39;&#39;-tris[2-naphthyl(phenyl)amino]triphenylamine (2-TNATA), Poly(ethylene oxide) and K2CF3SO3 showed white light emission with Commission internationale de l&#39;&#233;clairage (CIE) coordinates of (0.33, 0.43) and a Color Rendering Index (CRI) of Ra = 73 at an applied voltage of 3.5 V. Constant voltage measurements showed that the CIE coordinates of (0.27, 0.37), Ra of 67, and the emission color observed immediately after application of a voltage of 5 V were nearly unchanged and stable after 300 sec.

The authors present a method for fabricating stable white-light-emitting electrochemical cells utilizing emission from exciplexes formed between a blue-emitting fluorene polymer and aromatic amines.

Fremstilling af White Light-emitting elektrokemiske celler med Stable Emission fra Exciplexes

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active ...

Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser (laser-SARPES), and demonstrate a power of this technique for studying solid state physics. Laser-SARPES achieves two great capabilities. Firstly, by examining orbital selection rule of linearly polarized lasers, orbital selective excitation can be carried out in SAPRES experiment. Secondly, the technique can show full information of a variation of the spin quantum axis as a function of the light polarization. To demonstrate the power of the collaboration of these capabilities in laser-SARPES, we apply this technique for the investigations of spin-orbit coupled surface states of Bi2Se3. This technique affords to decompose spin and orbital components from the spin-orbit coupled wavefunctions. Moreover, as a representative advantage of using the direct spin detection collaborated with the polarization-variable laser, the technique unambiguously visualizes the light polarization dependence of the spin quantum axis in three-dimension. Laser-SARPES dramatically increases a capability of photoemission technique.

Here, we combine polarization-variable 7-eV laser with spin- and angle-resolved photoemission technique to visualize the spin-orbital coupling effect in solid states.

Eksperimentelle metoder for Spin - og vinkel-løst Photoemission spektroskopi kombineret med polarisering-variabel Laser

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser ...

A Silicon-tipped Fiber-optic Sensing Platform with High Resolution and Fast Response

In this article, we introduce an innovative and practically promising fiber-optic sensing platform (FOSP) that we proposed and demonstrated recently. This FOSP relies on a silicon Fabry-Perot interferometer (FPI) attached to the fiber end, referred to as Si-FOSP in this work. The Si-FOSP generates an interferogram determined by the optical path length (OPL) of the silicon cavity. Measurand alters the OPL and thus shifts the interferogram. Due to the unique optical and thermal properties of the silicon material, this Si-FOSP exhibits an advantageous performance in terms of sensitivity and speed. Furthermore, the mature silicon fabrication industry endows the Si-FOSP with excellent reproducibility and low cost toward practical applications. Depending on the specific applications, either a low-finesse or high-finesse version will be utilized, and two different data demodulation methods will be adopted accordingly. Detailed protocols for fabricating both versions of the Si-FOSP will be provided. Three representative applications and their according results will be shown. The first one is a prototype underwater thermometer for profiling the ocean thermoclines, the second one is a flow meter to measure flow speed in the ocean, and the last one is a bolometer used for monitoring exhaust radiation from magnetically confined high-temperature plasma.

This work reports an innovative silicon-tipped fiber-optic sensing platform (Si-FOSP) for high-resolution and fast-response measurement of a variety of physical parameters, such as temperature, flow, and radiation. Applications of this Si-FOSP span from oceanographic research, mechanical industry, to fusion energy research.

En silicium-tippes fiberoptisk Sensing Platform med høj opløsning og en hurtig reaktionstid

In this article, we introduce an innovative and practically promising fiber-optic sensing platform (FOSP) that we proposed and demonstrated recently. This ...