Part of the work has been performed in the project JEMSiP_3D, which is funded by the Public Authorities in France, Germany, Hungary, The Netherlands, Norway and Sweden, as well as by the ENIAC Joint Undertaking. The authors would like to thank the Dimes Technology Centre staff for processing support.

Dikkat: Kullanmadan önce ilgili tüm malzeme güvenlik bilgi formlarını (MSDS) danışın. Bu üretim işleminde kullanılan kimyasalların çeşitli akut olarak toksik ve kanserojen bulunmaktadır. Nanomalzemeler onların toplu meslektaşı ile karşılaştırıldığında ek tehlikeler olabilir. Mühendislik kontrolleri (davlumbaz) ve kişisel koruyucu ekipman (koruyucu gözlük, eldiven, temiz oda giysiler) kullanımı da dahil olmak üzere, ekipman, kimyasal madde veya Nanomalzemelerin ile çalışırken tüm uygun güvenlik uygulamalarını kullanın. Litografi 1. Hizalama Marker Tanımı <ol><li> Ya n ya da p-tipi doping ile tek taraflı cilalı endüstriyel notu Si (100) gofret ile başlayın. </li><li> Coat pozitif Fotorezist 1.4 mikron ile gofret. Uygun bir hızda (3500 rpm) soğuk levha, spin-kaplama üzerinde gofretin soğutulması ve ardından ışığa, yapışmasını teşvik etmek için 130 ° C&#39;da bir 90 sn heksametildisilazan (HMDS) tedavisi gerçekleştirin ve 90 sn, yumuşak bir fırındat 95 ° C. </li><li> Bir foto-litografi maskesi kullanma ve pozlama aracı Hizalama işaretlerini açığa pozlama dozu 120 mJ / cm 2. </li><li> Tek bir su birikintisi gelişim süreci gerçekleştirin. Karşı tedavi 100 ° C&#39;de geliştirici ve 90 sn sabit fırında kullanarak 60 sn gelişimi ardından 90 sn 115 ° C maruziyet sonrası fırında, gerçekleştirin. </li><li> Karşı delikler doğru boyutları ise incelemek için mikroskop kullanın. </li><li> Si klor plazma aşındırma kullanılarak 120 nm aşındırma. Bu kalınlık Bu çalışmada kullanılan poz aracının otomatik hizalama sistemleri için iyi bir kontrast sağlar. 20/40 sccm O 2 / CF 4, 5 mTorr, 60/500 W merdane / ICP RF gücü, Cl 2 80/40 sccm&#39;lik ardından 10 sn oksit atılım dağlama, / HBr: endüktif birleştiğinde plazma (ICP) kullanılarak, örneğin 60 mTorr, 20/500 W merdane / ICP RF gücü, 35 sn Si etch. </li><li> Işığa (1 kW, endpo 400 sccm O 2 kaldırmak için bir oksijen plazma striptizci kullanınint algılama ve 2 dakika overetch). Fotorezist aseton gibi, plazma, normal bir çözücü ile tedavi gibi kullanılamaz. </li><li> Gofret temizleyin. Su direnci 5 M? (Organik temiz) olana kadar ilk DI su içinde durulama izledi% 99 HNO 3, 10 dakika boyunca koydu. Su direnci 5 M? (Temiz metal) olana kadar 110 ° C&#39;de 65% HNO 3 içinde 10 dakika süreyle gofret, bu temiz sonra DI su ile çalkalayın. Gofret kurutmak için rinser kurutma makinesi kullanın. </li></ol> 2. Alt Metal ve Interlayers Dielektrik Biriktirme <ol><li> Aracılığıyla testin alt metal tabaka yatırmak için manyetik alanda sıçratma kullanın. Ti 500 nm, TİN 50 nm ve 100 nm Ti üç metal katman yığını tevdi edilmesi gerekmektedir. İlk Ti katman yığınının direncini azaltmak için, TiN CNT büyüme için gerçek bir destek katmanı, ve SİO2 tabakası 12 gravür, üst Ti plazma hasara karşı korumaktır TİN </sup&gt;. Ti 350 ° C&#39;lik bir yüzey sıcaklığında Ar-plazma ile saf Ti hedef kullanarak püskürtme gerçekleştirin. TiN reaktif sıçratma için 350 ° C taban sıcaklığında yine Ar ve N2 bir arada kullanabilirsiniz. </li><li> Plazma geliştirilmiş kimyasal buhar birikimi (PECVD) kullanarak SiO2 bir 1 um kalınlığında bir katman bırakır. Burada tetraetil ortosilikat (TEOS), 350 ° C&#39;lik bir sıcaklıkta ön levha olarak kullanılmaktadır. <ol><li> Uygun bir alet kullanarak SiO2 tabakasının kalınlığı, örneğin, bir reflektometre ve elipsometre edin. </li></ol></li><li> Kaplama uygun bir hızda (3500 rpm) soğuk levha, spin-kaplama üzerinde gofretin soğutulması ve ardından 130 ° C de 90 sn HMDS tedavisi ile başlayan pozitif fotorezist 1,4 um, gofret ve yumuşak bir 90 sn 95 ° C &#39;de fırında. </li><li> Bir foto-litografi maskesi ve pozlama aracını kullanarak, daha sonra SiO 2 t kazınmış olacak açıklıkların istenilen desen, maruzo hizalama işaretleri hizalanmış VIAS oluşturmak, pozlama dozu 140 mJ / cm 2. </li><li> 100 ° C&#39;de geliştirici ve 90 sn sabit fırında kullanarak 60 sn gelişimi ardından 90 sn 115 ° C maruziyet sonrası fırında ile başlayan tek bir su birikintisi geliştirme süreci, gerçekleştirin. </li><li> Karşı delikler doğru boyutları ve hizalama işaretleri ile bindirme doğruysa eğer incelemek için mikroskop kullanın. </li><li> Plazma SiO 2 kişi açıklıklar etch. Örneğin, C 2 F 6 ile bir triyot plazma yakıcısı kullanmak / CHF 3 36/144 sccm 180 mTor ve 300 W RF güçte. Eğer gerekli ise, zaman içinde 5% -10% için asitlenir üzerinde en aza indirmek için bir test gofret aşındırma oranı testleri. Not: Ti, bu flor kimyasında reaktif aşındırma dirençli olmasına rağmen, plazma uzun süre maruz kalma Ti tabakası fiziksel aşındırma ile sonuçlanacaktır. Ince tabaka plazmaya maruz kalırsa, bu negatif bir influen olacaktırCNT 12 büyümesi üzerine ce. Bu açıklıkların çok genişlemesi neden olacaktır olarak kısmen 4. sorunlu üst metalizasyonun yapma, ıslak aşındırma kullanmayın. </li><li> 60 saniye boyunca% 0.55 HF ıslak aşındırma yoluyla kurban Ti katmanı kaldırın. Su direnç kadar DI suyla durulayın gofret dağlama sonra 5 M? Ve gofret kurutmak için rinser kurutma makinesi kullanın. Not: Ti metalik gri ise Ti tabakası kazınmış eğer kontrol edilebilir bir mikroskop kullanarak, TiN tabakası altın-kahverengi renk olacaktır. </li></ol> 3. Catalyst Biriktirme ve CNT Büyüme <ol><li> Bir e-ışın buharlaştırıcı kullanılarak Co 5 nm buharlaşır. En az 2x10 -6 Torr kadar aşağı Pompa ve herhangi bir su filmi kaldırmak için yatırma önce vakum altında lambalar kullanılarak 60 ° C&#39;ye kadar ısıtın gofret. Fotoğraf karşı kontakt açıklıklar sağlamak üzere kullanılan SiO 2 kişi açıklıklar katalizörün kendini uyum sağlamak için gofret tutulur. </li><li> Kaldırasansör-off temas açıklıklar dışında Co. Co için, tetrahidrofuran (THF), düşük sıcaklıklarda iyi kalkış sonuçları ve büyüme sağladığı bulunmuştur. Daha önce Fe buharlaştırmadan sonra bir hareket başlangıcı için kullanılan N-metil-2-pirolidon (NMP), hasar bulunmuştur Co da böyle bir ölçüde herhangi hizalanmış CNT büyümesini önlemek için. 35 ° C&#39;de, THF ile bir ultrasonik banyoda 15 dakika için gofret koyun. 5 dakika boyunca DI suyla durulayın ve bir dönücü veya azot tabancası kullanarak kurutun. </li><li> Mikroskop altında gofret kontrol edin ve artıkları karşı kontrol edin. Kalıntıları elle kalıntılarını silip için kalkış amaçlı özel bir yumuşak pamuklu bir bez kullanın, isteğe bağlı olarak THF uzun bir ultrasonik tedavi gerçekleştirmek ve kalırsa. </li><li> Düşük basınçlı kimyasal buhar çöktürme (LPCVD) ile CNT büyüme gerçekleştirin. 50 sccm C 2 H 2 ekleyerek CNT büyüme izledi 80 mbar, 700 sccm&#39;lik H 2 ile 350 ° C&#39;de 8 dakika ön tavlama: Aşağıdaki tarifi kullanın. 350 ° C&#39;de, 60büyüme dakika yaklaşık 1 um CNT verir. Gerekirse ayarlamak için bir test büyüme SiO 2 tabaka olarak aynı kalınlıkta olmalıdır yükseklik, gerçekleştirin. Reaktörü soğutun ve N 2 kullanarak temizlemek. </li><li> Ya da bir kesite hazırlanmasıyla 45 ° eğim altındaki çıkış bölümünün içinde CNT yüksekliğini kontrol etmek için bir tarama elektron mikroskopu kullanın. </li><li> CNT 18 kristalliğini belirlemek için Raman spektroskopisi kullanarak örnekleri inceleyin. </li></ol> 4. Borda Metalleştirme <ol><li> Üst metal yatırmak için manyetik alanda sıçratma kullanın. Ti CNT 19 temas etmek için iyi bir metal gibi, birinci vakum bozmadan Al (% 1 Si) 2 um, ardından Ti 100 nm, saçılırlar. </li><li> Kaplama 3000 rpm&#39;de soğuk levha, spin-kaplama üzerinde gofretin soğutulması ve ardından 130 ° C de 90 sn HMDS tedavisi ile başlayan yüksek bir viskoziteye sahip pozitif fotorezist 3,1 um, ve 90 sn, yumuşak fırında de gofret 95° C. </li><li> Bir foto-litografi maskesi ve pozlama aracını kullanarak hizalama işaretleri hizalanmış üst metal deseni, maruz kalma dozu 420 mJ / cm 2, -1 odağı maruz. </li><li> Tek bir su birikintisi gelişim süreci gerçekleştirin. Bu, 100 ° C de bir geliştirici ve 90 saniye sabit fırında kullanılarak 60 sn geliştirilmesi yolu ile, ardından 90 saniye 115 ° C maruziyet sonrası fırında ile başlar. </li><li> Karşı çizgiler doğru boyutları ve işaretlere bindirme doğruysa eğer incelemek için mikroskop kullanın. </li><li> Klor plazma aşındırma kullanarak Ti / Al yığını etch. Endüktif birleştiğinde plazma kullanılarak Örneğin: 30/40 sccm Cl 2 / HBr, 5 mTorr, uç nokta tespiti ve% 80 overetch ile 40/500 W Platen / ICP RF güç 15/30 sccm Cl 2 / HBr&#39;nin kullanarak. </li><li> Işığa (1 kW, uç nokta tespiti ve 2 dakika overetch 400 sccm O 2) kaldırmak için bir oksijen plazma striptizci kullanın. Metal kapsamı tam değilse (yani, iğne delikleri etrafında vardırCNT) CNT plazma hasar görmesini önlemek için, ışığa kaldırmak için bir organik çözücü (örneğin NMP) kullanın. </li><li> Gofret temizleyin. Su direnci 5 M? (Organik temiz) olduğu kadar DI su ile çalkalayın% 99 HNO 3, 10 dakika boyunca koyun. Gofret kurutmak için rinser kurutma makinesi kullanın. </li></ol> 5. Ölçümler <ol><li> Gofret üst metalleşme kontrol etmek için üreticinin talimatlarına göre taramalı elektron mikroskobu kullanın. Not:. Şekil 3 &#39;de gösterildiği gibi gofret mekanik görüntü ile sonuçlanan 90 °&#39; lik bir eğim kullanılarak örnek yoluyla tam CNT kontrol etmek için bölünebilen Gerektiğinde numuneleri, elektriksel olarak iletken olduğu için ek bir tedavi adım kullanılmak üzere ve Numuneler doğrudan SEM içine monte edilebilir. Genel olarak, 15 ya da 20 kV yüksek ivmeli voltajının, ancak SİO2 tabakası eğer çok fazla Bu azaltılabilir t kadar şarj edilir5 kV o. </li><li> 4-nokta gerçekleştirme Şekil 1 ve Vollebregt ve ark., 16 de tarif edildiği gibi bir yarı-iletken bir parametre analizörü ile bir arada bir prob istasyonu kullanılarak prob IV ölçümleri. Not: Bir ara bağlantısı üzerindeki potansiyel damla ideal küçük Normalde -0.5 V 0.5 bir gerilim süpürme, yeterlidir. 4-noktalı prob kurulumu kullanarak prob iğne ve kurulum tel dirençler temas direnci ihmal edilmiştir. </li></ol>

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The authors have nothing to disclose.

Şekil 1, bu çalışmada imal yapısının şematik genel bakışını gösterir ve bu 4-nokta prob ölçümleri için kullanıldı. Potansiyel hiçbir akım taşıyan problar ile ölçülür gibi, merkezi CNT demeti ve metal olan kişiler üzerinde tam potansiyel damla (VH -V L) ölçülebilir. Büyük çaplı CNT demetleri akım zorlama problar için toplam direncini azaltmak ve merkezi CNT paket üzerindeki potansiyel düşüş maksimize etmek için, kontak pedleri gelen alt Ti...

Bakır ve tungsten, şu anda devlet-of-the-art çok-büyük ölçekli entegrasyon (VLSI) teknolojisinde ara bağlantı için kullanılan metaller, güvenilirlik ve elektrik iletkenliği 1 açısından fiziksel sınırlarının yaklaşıyor. Aşağı-ölçekleme transistörler genellikle performansı artırır iken, aslında direnç ve interconnect&#39;lerdeki akım yoğunluğunu arttırır. Bu gecikme ve güç tüketimi 2 açısından entegre devre (IC) bir performans hakim ara bağlantı ile sonuçlanmıştır. Karbon nanotüpler (CNT) dikey interconnet CNT olarak (yollar,) kolayca 3 dikey büyümüş olabilir özellikle, Cu ve W madensel alternatif olarak ileri sürülmüştür. CNT Cu 4 den 1000 katı daha yüksek akım yoğunluğu bir ile tamamen mükemmel elektriksel güvenilirlik gösterilmiştir. Ayrıca, CNT yüzey ve tane sınırı saçılma muzdarip değil, hangi r artıyornanometre ölçeğinde 5 de Cu esistivity. Son olarak, CNT VLSI fiş ısı yönetimi yardımcı olabilir mükemmel termal iletken 6, olduğu gösterilmiştir. VLSI teknolojisi CNT başarılı entegrasyon için CNT büyüme süreçleri yarı iletken fabrikasyon uyumlu yapılmış olması önemlidir. Bu malzeme ve büyük ölçekli imalat uyumlu ve ölçeklenebilir kabul edilir ekipman kullanılarak CNT (&lt;400 ° C) düşük sıcaklık büyümesini gerektirir. CNT Test yolların bir çok örneği literatürde 7,8,9,10,11,12,13,14 gösterilmiştir olsa da, bunların çoğu IC kontaminant 15 imalat olarak kabul edilir, katalizör olarak Fe kullanımı. Bunun yanı sıra, bu çalışmaların birçoğunda kullanılan büyüme sıcaklığı 400 ° C üst sınırının çok daha yüksektir. Tercihen CNT hatta modern düşük κ yalıtkanların veya esnek ile entegrasyon sağlamak amacıyla, 350 ° C&#39;nin altında yetiştirilen olmalıdıryüzeyler. Burada katalizör 16 VR ile 350 ° C kadar düşük sıcaklıklarda CNT yetiştirmek için ölçeklenebilir bir yöntem sunulmaktadır. Bu yöntem, entegre devreler dik olarak sıralanmaktadır CNT oluşan farklı elektrik yapıların imal edilmesi, süper kondansatör ve alan emisyon cihazlara ara-bağlantısı ve elektrotların arasında değişen için ilgi çekmektedir. TiN sık kullanılan bariyer malzemesi 7 ise Co katalizör metal genellikle, silisid en 17 imalatı için IC imalat alanlarında kullanılmaktadır. Ayrıca, yalnızca standart yarıiletken imalat teknikleri kullanarak CNT Test VIAS imal edilmesi için bir işlem ortaya koymaktadır. Bu grubu, CNT testi yollar, elektron mikroskobu (SEM) ve Raman spektroskopisi ve elektriksel karakterize tarayarak tarafından denetlenir, imal edilir.

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			<td style="width:291px;">Comments/Description</td>
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			<td height="21" style="height:21px;width:307px;">Si (100) wafer 4&#34;</td>
			<td style="width:188px;">International Wafer Service</td>
			<td style="width:119px;"></td>
			<td>Resisitivity: 2-5 m&#937;-cm, thickness: 525 &#181;m&#160;</td>
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			<td height="21" style="height:21px;width:307px;">Ti-sputtertarget (99.995 % purity)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;width:307px;">Al (1% Si)-sputtertarget (99.999 % purity)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">Co (99.95 % purity)</td>
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			<td style="width:188px;">Dow Electronic Materials</td>
			<td style="width:119px;"></td>
			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;width:307px;">MF-322 developer</td>
			<td style="width:188px;">Dow Electronic Materials</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">HNO3 (99.9 %)</td>
			<td style="width:188px;">KMG Ultra Pure Chemicals</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">HNO3 (69.5%)</td>
			<td style="width:188px;">KMG Ultra Pure Chemicals</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">HF 0.55%</td>
			<td style="width:188px;">Honeywell</td>
			<td style="width:119px;"></td>
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			<td height="21" style="height:21px;width:307px;">Tetrahydrofuran</td>
			<td style="width:188px;">JT Baker</td>
			<td style="width:119px;"></td>
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			<td height="21" style="height:21px;width:307px;">Acetone</td>
			<td style="width:188px;">Sigma-Aldrich</td>
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			<td height="21" style="height:21px;width:307px;">ECI3027 positive photoresist</td>
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			<td height="21" style="height:21px;width:307px;">Tetraethyl orthosilicate (TEOS)</td>
			<td style="width:188px;">Praxair</td>
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			<td style="width:188px;">Company</td>
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			<td height="21" style="height:21px;width:307px;">N2 (99.9990%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">O2 (99.9999%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;width:307px;">CF4 (99.9970%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">CL2 (99.9900%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">HBr (99.9950%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
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			<td height="21" style="height:21px;width:307px;">Ar (99.9990%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
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			<td height="21" style="height:21px;width:307px;">C2F6 (99.9990%)</td>
			<td style="width:188px;">Praxair</td>
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			<td height="21" style="height:21px;width:307px;">CHF3 (99.9950%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:307px;">H2 (99.9950%)</td>
			<td style="width:188px;">Praxair</td>
			<td style="width:119px;"></td>
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			<td height="21" style="height:21px;width:307px;">C2H2 (99.6000%)</td>
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			<td height="21" style="height:21px;width:307px;">SPTS &#937;mega 201 plasma etcher</td>
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			<td>Used for Si and metal etching</td>
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			<td height="21" style="height:21px;width:307px;">Novellus Concept One PECVD</td>
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			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;width:307px;">Drytek 384T plasma etcher</td>
			<td style="width:188px;">LAM</td>
			<td style="width:119px;"></td>
			<td>Used for oxide etching</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:307px;">CHA Solution e-beam evaporator</td>
			<td style="width:188px;">CHA</td>
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			<td></td>
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			<td height="21" style="height:21px;width:307px;">AIXTRON BlackMagic Pro CVD tool</td>
			<td style="width:188px;">AIXTRON</td>
			<td style="width:119px;"></td>
			<td>Carbon nanotube growth</td>
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			<td height="21" style="height:21px;width:307px;">Tepla 300</td>
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			<td>Resist plasma stripper</td>
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			<td style="width:188px;">Agilent</td>
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			<td style="width:188px;">Cascade Microtech</td>
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fabrication of low temperature carbon nanotube vertical interconnects compatible with semiconductor technology

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive thin-films. Due to the low growth temperature, the process allows integration with modern low-&#954; dielectrics and some flexible substrates. The process is compatible with standard semiconductor fabrication, and a method for the fabrication of electrical 4-point probe test structures for vertical interconnect test structures is presented. Using scanning electron microscopy the morphology of the CNT bundles is investigated, which demonstrates vertical alignment of the CNT and can be used to tune the CNT growth time. With Raman spectroscopy the crystallinity of the CNT is investigated. It was found that the CNT have many defects, due to the low growth temperature. The electrical current-voltage measurements of the test vertical interconnects displays a linear response, indicating good ohmic contact was achieved between the CNT bundle and the top and bottom metal electrodes. The obtained resistivities of the CNT bundle are among the average values in the literature, while a record-low CNT growth temperature was used.

Bu çalışmada kullanılan ölçüm yapısının tasarımı, Şekil 1 &#39;de bulunabilir. Prob, tel dirençleri atlatılabilir olarak CNT demeti direnci ve metal CNT dirençleri ölçümü doğru olarak belirlenebilir, böyle bir yapının kullanılması suretiyle. Demetin direnci CNT demetinin kalitesi ve yoğunluğu için bir ölçüdür. Farklı uzunluklarda temas direnci demetleri belirlemek için ölçülür. 45 ° hızıyla metalle önce üst alınan 60 dakika boyunc...

Watch this Scientific Journal Video about Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology at JoVE.com

Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology

A method for the growth of low temperature vertically-aligned carbon nanotubes, and the subsequent fabrication of vertical interconnect electrical test structures using semiconductor fabrication is presented.

Yarıiletken Teknolojisi ile uyumlu Düşük Sıcaklık Karbon Nanotüp Dikey Bağlantıları Fabrikasyon

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive ...

fabrication-low-temperature-carbon-nanotube-vertical-interconnects

Research

JoVE Journal

Engineering

7.6K Görüntüleme.  Delft University of Technology. A method for the growth of low temperature vertically-aligned carbon nanotubes, and the subsequent fabrication of vertical interconnect electrical test structures using semiconductor fabrication is presented.

Video: Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology

Fabrication, Densification, and Replica Molding of 3D Carbon Nanotube Microstructures

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip devices, and their applications. In particular, capabilities for cost-effective fabrication of polymer microstructures were transformed by the advent of soft lithography and other micromolding techniques 1, 2, and this led a revolution in applications of microfabrication to biomedical engineering and biology. Nevertheless, it remains challenging to fabricate microstructures with well-defined nanoscale surface textures, and to fabricate arbitrary 3D shapes at the micro-scale. Robustness of master molds and maintenance of shape integrity is especially important to achieve high fidelity replication of complex structures and preserving their nanoscale surface texture. The combination of hierarchical textures, and heterogeneous shapes, is a profound challenge to existing microfabrication methods that largely rely upon top-down etching using fixed mask templates. On the other hand, the bottom-up synthesis of nanostructures such as nanotubes and nanowires can offer new capabilities to microfabrication, in particular by taking advantage of the collective self-organization of nanostructures, and local control of their growth behavior with respect to microfabricated patterns. 
Our goal is to introduce vertically aligned carbon nanotubes (CNTs), which we refer to as CNT "forests", as a new microfabrication material. We present details of a suite of related methods recently developed by our group: fabrication of CNT forest microstructures by thermal CVD from lithographically patterned catalyst thin films; self-directed elastocapillary densification of CNT microstructures; and replica molding of polymer microstructures using CNT composite master molds. In particular, our work shows that self-directed capillary densification ("capillary forming"), which is performed by condensation of a solvent onto the substrate with CNT microstructures, significantly increases the packing density of CNTs. This process enables directed transformation of vertical CNT microstructures into straight, inclined, and twisted shapes, which have robust mechanical properties exceeding those of typical microfabrication polymers. This in turn enables formation of nanocomposite CNT master molds by capillary-driven infiltration of polymers. The replica structures exhibit the anisotropic nanoscale texture of the aligned CNTs, and can have walls with sub-micron thickness and aspect ratios exceeding 50:1. Integration of CNT microstructures in fabrication offers further opportunity to exploit the electrical and thermal properties of CNTs, and diverse capabilities for chemical and biochemical functionalization 3.

We present methods for fabrication of patterned microstructures of vertically aligned carbon nanotubes (CNTs), and their use as master molds for production of polymer microstructures with organized nanoscale surface texture. The CNT forests are densified by condensation of solvent onto the substrate, which significantly increases their packing density and enables self-directed formation of 3D shapes.

3D Karbon Nanotube mikroyapılar, Üretimi, Yoğunlaştırma ve Replica Kalıp

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip ...

Mühendislik

Dry Oxidation and Vacuum Annealing Treatments for Tuning the Wetting Properties of Carbon Nanotube Arrays

In this article, we describe a simple method to reversibly tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays. Here, CNT arrays are defined as densely packed multi-walled carbon nanotubes oriented perpendicular to the growth substrate as a result of a growth process by the standard thermal chemical vapor deposition (CVD) technique.1,2 These CNT arrays are then exposed to vacuum annealing treatment to make them more hydrophobic or to dry oxidation treatment to render them more hydrophilic. The hydrophobic CNT arrays can be turned hydrophilic by exposing them to dry oxidation treatment, while the hydrophilic CNT arrays can be turned hydrophobic by exposing them to vacuum annealing treatment. Using a combination of both treatments, CNT arrays can be repeatedly switched between hydrophilic and hydrophobic.2 Therefore, such combination show a very high potential in many industrial and consumer applications, including drug delivery system and high power density supercapacitors.3-5
The key to vary the wettability of CNT arrays is to control the surface concentration of oxygen adsorbates. Basically oxygen adsorbates can be introduced by exposing the CNT arrays to any oxidation treatment. Here we use dry oxidation treatments, such as oxygen plasma and UV/ozone, to functionalize the surface of CNT with oxygenated functional groups. These oxygenated functional groups allow hydrogen bond between the surface of CNT and water molecules to form, rendering the CNT hydrophilic. To turn them hydrophobic, adsorbed oxygen must be removed from the surface of CNT. Here we employ vacuum annealing treatment to induce oxygen desorption process. CNT arrays with extremely low surface concentration of oxygen adsorbates exhibit a superhydrophobic behavior.

This article describes a simple method to fabricate vertically aligned carbon nanotube arrays by CVD and to subsequently tune their wetting properties by exposing them to vacuum annealing or dry oxidation treatment.

Karbon Nanotube Dizilerin Islatma Özellikleri Tuning Tedaviler Tavlama Kuru Oksidasyon ve Vakum

In this article, we describe a simple method to reversibly  tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays.  Here, CNT ...

Synthesis and Functionalization of Nitrogen-doped Carbon Nanotube Cups with Gold Nanoparticles as Cork Stoppers

Nitrogen-doped carbon nanotubes consist of many cup-shaped graphitic compartments termed as nitrogen-doped carbon nanotube cups (NCNCs). These as-synthesized graphitic nanocups from chemical vapor deposition (CVD) method were stacked in a head-to-tail fashion held only through noncovalent interactions. Individual NCNCs can be isolated out of their stacking structure through a series of chemical and physical separation processes. First, as-synthesized NCNCs were oxidized in a mixture of strong acids to introduce oxygen-containing defects on the graphitic walls. The oxidized NCNCs were then processed using high-intensity probe-tip sonication which effectively separated the stacked NCNCs into individual graphitic nanocups. Owing to their abundant oxygen and nitrogen surface functionalities, the resulted individual NCNCs are highly hydrophilic and can be effectively functionalized with gold nanoparticles (GNPs), which preferentially fit in the opening of the cups as cork stoppers. These graphitic nanocups corked with GNPs may find promising applications as nanoscale containers and drug carriers.

We discussed the synthesis of individual graphitic nanocups using a series of techniques including chemical vapor deposition, acid oxidation and probe-tip sonication. By citrate reduction of HAuCl4, the graphitic nanocups were effectively corked with gold nanoparticles due to the chemically reactive edges of the cups.

Mantar Tıpa olarak Altın Nanopartiküller ile Azot-katkılı Karbon Nanotube Bardaklar sentezi ve fonksiyonlandırmalar

Nitrogen-doped carbon  nanotubes consist of many cup-shaped graphitic compartments termed as  nitrogen-doped carbon nanotube cups (NCNCs).  These ...

Writing and Low-Temperature Characterization of Oxide Nanostructures

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions. Oxide interfaces exhibit a wide range of properties that can be controlled include conduction, piezoelectric behavior, ferromagnetism, superconductivity and nonlinear optical properties. Recently, methods for controlling these properties at extreme nanoscale dimensions have been discovered and developed. Here are described explicit step-by-step procedures for creating LaAlO3/SrTiO3 nanostructures using a reversible conductive atomic force microscopy technique. The processing steps for creating electrical contacts to the LaAlO3/SrTiO3 interface are first described. Conductive nanostructures are created by applying voltages to a conductive atomic force microscope tip and locally switching the LaAlO3/SrTiO3 interface to a conductive state. A versatile nanolithography toolkit has been developed expressly for the purpose of controlling the atomic force microscope (AFM) tip path and voltage. Then, these nanostructures are placed in a cryostat and transport measurements are performed. The procedures described here should be useful to others wishing to conduct research in oxide nanoelectronics.

Oxide nanostructures provide new opportunities for science and technology. The interfacial conductivity between LaAlO3 and SrTiO3 can be controlled with near-atomic precision using a conductive atomic force microscopy technique. The protocol for creating and measuring conductive nanostructures at LaAlO3/SrTiO3 interfaces is demonstrated.

Yazma ve Oksit Nanoyapıların Düşük Sıcaklık Karakterizasyonu

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions.  Oxide ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

Ohmik İletişim Fabrikasyon bir Odaklı iyon Işın Tekniği ve Elektriksel Karakterizasyonu Katmanı Yarıiletken Nanoyapıların için kullanma

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

Yeni Malzemelerin Düşük sıcaklık Magnetotransport Ölçüm İleri Deneysel Yöntemler

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

Precision Milling of Carbon Nanotube Forests Using Low Pressure Scanning Electron Microscopy

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning electron microscope (ESEM) operating with a low pressure water vapor ambient. In this technique, a portion of the electron beam interacts with the water vapor in the vicinity of the CNT sample, dissociating the water molecules into hydroxyl radicals and other species by radiolysis. The remainder of the electron beam interacts with the CNT forest sample, making it susceptible to oxidation from the chemical products of radiolysis. This technique may be used to trim a selected region of an individual CNT, or it may be used to remove hundreds of cubic microns of material by adjusting ESEM parameters. The machining resolution is similar to the imaging resolution of the ESEM itself. The technique produces only small quantities of carbon residue along the boundaries of the cutting zone, with minimal effect on the native structural morphology of the CNT forest.

Low pressure scanning electron microscopy in a water vapor ambient is used to machine nanoscale to microscale features in carbon nanotube forests.

Alçak Basınç Taramalı Elektron Mikroskobu kullanılarak Karbon Nanotüp Ormanlar Hassas freze

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

tarafından Nano yapılı yitriya stabilize-Zirkonyum (YSZ) iskelelerinin Yüksek Sıcaklık Fabrikasyon<em&gt; Situ</em&gt; Karbon şablonu Kserojeller

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Fabrication of 3D Carbon Microelectromechanical Systems (C-MEMS)

A wide range of carbon sources are available in nature, with a variety of micro-/nanostructure configurations. Here, a novel technique to fabricate long and hollow glassy carbon microfibers derived from human hairs is introduced. The long and hollow carbon structures were made by the pyrolysis of human hair at 900 &#176;C in a N2 atmosphere. The morphology and chemical composition of natural and pyrolyzed human hairs were investigated using scanning electron microscopy (SEM) and electron-dispersive X-ray spectroscopy (EDX), respectively, to estimate the physical and chemical changes due to pyrolysis. Raman spectroscopy was used to confirm the glassy nature of the carbon microstructures. Pyrolyzed hair carbon was introduced to modify screen-printed carbon electrodes ; the modified electrodes were then applied to the electrochemical sensing of dopamine and ascorbic acid. Sensing performance of the modified sensors was improved as compared to the unmodified sensors. To obtain the desired carbon structure design, carbon micro-/nanoelectromechanical system (C-MEMS/C-NEMS) technology was developed. The most common C-MEMS/C-NEMS fabrication process consists of two steps: (i) the patterning of a carbon-rich base material, such as a photosensitive polymer, using photolithography; and (ii) carbonization through the pyrolysis of the patterned polymer in an oxygen-free environment. The C-MEMS/NEMS process has been widely used to develop microelectronic devices for various applications, including in micro-batteries, supercapacitors, glucose sensors, gas sensors, fuel cells, and triboelectric nanogenerators. Here, recent developments of a high-aspect ratio solid and hollow carbon microstructures with SU8 photoresists are discussed. The structural shrinkage during pyrolysis was investigated using confocal microscopy and SEM. Raman spectroscopy was used to confirm the crystallinity of the structure, and the atomic percentage of the elements present in the material before and after pyrolysis was measured using EDX.

Fabrication of 3D Carbon Microelectromechanical Systems C-MEMS

Long and hollow glassy carbon microfibers were fabricated based on the pyrolysis of a natural product, human hair. The two fabrication steps of carbon microelectromechanical and carbon nanoelectromechanical systems, or C-MEMS and C-NEMS, are: (i) photolithography of a carbon-rich polymer precursor and (ii) pyrolysis of the patterned polymer precursor.

3D Karbon Mikroelektromekanik Sistemlerin (C-MEMS) İmalatı

A wide range of carbon sources are available in nature, with a variety of micro-/nanostructure configurations. Here, a novel technique to fabricate long ...

Flow-assisted Dielectrophoresis: A Low Cost Method for the Fabrication of High Performance Solution-processable Nanowire Devices

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of nanowires. DEP is used for nanowire analysis, characterization, and for solution-based fabrication of semiconducting devices. The method works by applying an alternating electric field between metallic electrodes. The nanowire formulation is then dropped onto the electrodes which are on an inclined surface to create a flow of the formulation using gravity. The nanowires then align along the gradient of the electric field and in the direction of the liquid flow. The frequency of the field can be adjusted to select nanowires with superior conductivity and lower trap density. 
In this work, flow-assisted DEP is used to create nanowire field effect transistors. Flow-assisted DEP has several advantages: it allows selection of nanowire electrical properties; control of nanowire length; placement of nanowires in specific areas; control of orientation of nanowires; and control of nanowire density in the device. 
The technique can be expanded to many other applications such as gas sensors and microwave switches. The technique is efficient, quick, reproducible, and it uses a minimal amount of dilute solution making it ideal for the testing of novel nanomaterials. Wafer scale assembly of nanowire devices can also be achieved using this technique, allowing large numbers of samples for testing and large-area electronic applications.

In this paper, flow assisted dielectrophoresis is demonstrated for the self-assembly of nanowire devices. The fabrication of a silicon nanowire field effect transistor is shown as an example.

Akış yoluyla Dielectrophoresis: Yüksek performanslı çözüm processable Nanowire cihazları imalatı için düşük maliyetli bir yöntem

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of ...